+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 04skc0008p-1 started at 11:17:31 on 06-Aug-2008 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 04skc0008p-1 in P-1 CELL 0.71073 7.8263 9.6552 17.8962 101.635 94.082 92.688 ZERR 2.00 0.0015 0.0019 0.0016 0.010 0.011 0.011 LATT 1 SFAC C H N O BR UNIT 38 84 4 26 2 V = 1318.57 F(000) = 618.0 Mu = 1.62 mm-1 Cell Wt = 1172.91 Rho = 1.477 MERG 2 OMIT -3.00 55.00 OMIT -1 -1 1 OMIT -1 1 1 OMIT -1 2 4 SHEL 7 0.77 DFIX 0.84 0.02 O1W H1W O1W H2W DANG 1.35 0.02 H1W H2W HTAB O3 O4A HTAB O33 O34A EQIV_$1 x, y+1, z+1 HTAB O1A O34B_$1 EQIV_$2 -x+1, -y+2, -z+1 HTAB O2 Br1_$2 HTAB N41 O2_$2 HTAB N41 O1B_$2 EQIV_$3 -x, -y+1, -z+1 HTAB O3 O1W_$3 EQIV_$4 x-1, y, z HTAB O4B O1B_$4 HTAB O1W Br1_$4 EQIV_$5 x+1, y, z HTAB O31A O34A_$5 EQIV_$6 -x+2, -y+1, -z HTAB O32 O33_$6 HTAB O33 O31A_$6 EQIV_$7 -x+1, -y+1, -z+1 HTAB O1W Br1_$7 FMAP 2 PLAN 10 SIZE 0.08 0.10 0.10 ACTA BOND $H WGHT 0.04980 1.25890 L.S. 4 TEMP -153.00 FVAR 0.57171 MOLE 1 C1 1 0.340642 1.122433 0.725223 11.00000 0.01914 0.01349 = 0.01917 0.00013 0.00025 0.00151 C2 1 0.155659 1.114131 0.691277 11.00000 0.01462 0.01762 = 0.01385 0.00049 -0.00071 0.00204 AFIX 13 H2 2 0.103285 1.205616 0.710773 11.00000 -1.20000 AFIX 0 C3 1 0.055863 0.993990 0.716470 11.00000 0.01549 0.01795 = 0.01703 0.00081 0.00067 0.00408 AFIX 13 H3 2 0.069277 1.011384 0.773647 11.00000 -1.20000 AFIX 0 C4 1 -0.133723 0.989472 0.691681 11.00000 0.01796 0.01846 = 0.01567 0.00451 0.00181 0.00397 O1A 4 0.354927 1.169726 0.797467 11.00000 0.01557 0.03764 = 0.01731 -0.00470 -0.00294 0.00268 AFIX 147 H1 2 0.454876 1.159667 0.815135 11.00000 -1.50000 AFIX 0 O1B 4 0.457794 1.085143 0.684293 11.00000 0.01598 0.02733 = 0.01828 0.00090 0.00103 0.00405 O2 4 0.141962 1.085918 0.610555 11.00000 0.02051 0.02066 = 0.01394 0.00326 -0.00148 0.00047 AFIX 147 H2O 2 0.164292 1.161071 0.595352 11.00000 -1.50000 AFIX 0 O3 4 0.128246 0.865609 0.687846 11.00000 0.01860 0.01525 = 0.03241 0.00089 -0.00203 0.00213 AFIX 147 H3O 2 0.049952 0.804356 0.667445 11.00000 -1.50000 AFIX 0 O4A 4 -0.211992 0.885565 0.653970 11.00000 0.02054 0.02065 = 0.03550 0.00094 -0.00601 0.00041 O4B 4 -0.201940 1.110141 0.717575 11.00000 0.01354 0.02346 = 0.02759 -0.00425 -0.00001 0.00197 AFIX 147 H4B 2 -0.308006 1.101854 0.705082 11.00000 -1.50000 AFIX 0 MOLE 2 C22A 1 0.400184 0.404900 0.278406 11.00000 0.03562 0.02942 = 0.01867 0.00475 0.00681 0.00223 AFIX 23 H22A 2 0.321322 0.335078 0.294328 11.00000 -1.20000 H22B 2 0.506138 0.417205 0.313367 11.00000 -1.20000 AFIX 0 C22B 1 0.288485 0.318671 0.141503 11.00000 0.02741 0.03659 = 0.02287 0.01188 -0.00420 0.00393 AFIX 23 H22C 2 0.324717 0.281640 0.089728 11.00000 -1.20000 H22D 2 0.238307 0.410648 0.140705 11.00000 -1.20000 AFIX 0 C22C 1 0.529528 0.207419 0.199778 11.00000 0.02712 0.02307 = 0.03078 0.01067 0.00058 0.00638 AFIX 23 H22E 2 0.444707 0.139977 0.214016 11.00000 -1.20000 H22F 2 0.625562 0.226065 0.240293 11.00000 -1.20000 AFIX 0 C22D 1 0.566589 0.448117 0.170444 11.00000 0.03466 0.02514 = 0.02097 0.00590 0.00843 -0.00223 AFIX 23 H22G 2 0.586104 0.409279 0.116381 11.00000 -1.20000 H22H 2 0.509778 0.538044 0.172114 11.00000 -1.20000 AFIX 0 C23A 1 0.317238 0.544638 0.288072 11.00000 0.05589 0.03300 = 0.03532 0.00058 0.02000 0.01148 AFIX 137 H23A 2 0.400908 0.618621 0.280918 11.00000 -1.50000 H23B 2 0.277879 0.569155 0.339596 11.00000 -1.50000 H23C 2 0.219043 0.536916 0.249981 11.00000 -1.50000 AFIX 0 C23B 1 0.149942 0.216555 0.158122 11.00000 0.02543 0.06715 = 0.03832 0.02349 -0.00789 -0.00907 AFIX 137 H23D 2 0.196407 0.123729 0.157027 11.00000 -1.50000 H23E 2 0.053001 0.207126 0.119263 11.00000 -1.50000 H23F 2 0.110896 0.252826 0.208814 11.00000 -1.50000 AFIX 0 C23C 1 0.597729 0.138341 0.125047 11.00000 0.04468 0.02313 = 0.04439 0.00395 0.00985 0.00919 AFIX 137 H23G 2 0.503040 0.116122 0.084816 11.00000 -1.50000 H23H 2 0.650609 0.050841 0.131139 11.00000 -1.50000 H23I 2 0.683670 0.203358 0.110829 11.00000 -1.50000 AFIX 0 C23D 1 0.738913 0.480141 0.216405 11.00000 0.03888 0.03896 = 0.02875 0.00003 0.00353 -0.01805 AFIX 137 H23J 2 0.721706 0.522062 0.269733 11.00000 -1.50000 H23K 2 0.808887 0.546888 0.194894 11.00000 -1.50000 H23L 2 0.797710 0.392205 0.214342 11.00000 -1.50000 AFIX 0 N21 3 0.445926 0.344402 0.197730 11.00000 0.02305 0.02009 = 0.01601 0.00429 0.00088 0.00246 MOLE 3 C31 1 1.152179 0.252326 -0.063321 11.00000 0.01930 0.03202 = 0.01721 -0.00624 0.00193 0.00589 C32 1 0.968569 0.265384 -0.094114 11.00000 0.01977 0.03318 = 0.01968 -0.00169 0.00011 0.00284 AFIX 13 H32 2 0.940613 0.185732 -0.139238 11.00000 -1.20000 AFIX 0 C33 1 0.847661 0.246040 -0.034205 11.00000 0.02164 0.02656 = 0.01927 -0.00334 -0.00222 0.00158 AFIX 13 H33 2 0.863890 0.152269 -0.019967 11.00000 -1.20000 AFIX 0 C34 1 0.664928 0.248279 -0.068075 11.00000 0.01856 0.02986 = 0.01864 -0.00038 -0.00095 -0.00074 O31A 4 1.251751 0.366496 -0.059646 11.00000 0.01364 0.03113 = 0.02871 -0.00049 -0.00006 0.00546 AFIX 147 H31A 2 1.354602 0.348110 -0.052020 11.00000 -1.50000 AFIX 0 O31B 4 1.196373 0.146010 -0.043785 11.00000 0.02425 0.03043 = 0.03583 -0.00078 0.00454 0.00170 O32 4 0.939425 0.394005 -0.119102 11.00000 0.02703 0.03090 = 0.02909 0.00732 -0.00282 0.00109 AFIX 147 H32O 2 0.980789 0.463020 -0.085204 11.00000 -1.50000 AFIX 0 O33 4 0.882874 0.354766 0.031749 11.00000 0.01805 0.02436 = 0.01443 -0.00365 -0.00028 0.00240 AFIX 147 H33O 2 0.800340 0.407569 0.036487 11.00000 -1.50000 AFIX 0 O34A 4 0.573358 0.336066 -0.035148 11.00000 0.01452 0.03190 = 0.02807 -0.00392 0.00018 0.00359 O34B 4 0.623841 0.152366 -0.128191 11.00000 0.02514 0.03523 = 0.02547 -0.00057 -0.00192 -0.00015 MOLE 4 N41 3 0.645946 1.129433 0.463026 11.00000 0.01874 0.01676 = 0.01443 -0.00002 0.00247 -0.00037 AFIX 13 H41 2 0.673842 1.061598 0.421688 11.00000 -1.20000 AFIX 0 C42 1 0.488874 1.073682 0.492898 11.00000 0.02280 0.02163 = 0.02407 0.00576 0.00562 0.00110 AFIX 23 H42A 2 0.388992 1.071520 0.455395 11.00000 -1.20000 H42B 2 0.465839 1.137654 0.541259 11.00000 -1.20000 AFIX 0 C43 1 0.796829 1.158539 0.519795 11.00000 0.02532 0.03793 = 0.02630 0.00450 -0.00563 -0.00294 AFIX 137 H43A 2 0.768985 1.226819 0.565015 11.00000 -1.50000 H43B 2 0.893619 1.197838 0.497171 11.00000 -1.50000 H43C 2 0.827837 1.070240 0.534807 11.00000 -1.50000 AFIX 0 C44 1 0.604269 1.259385 0.434262 11.00000 0.03058 0.02231 = 0.03405 0.01055 0.00672 0.00527 AFIX 137 H44A 2 0.568028 1.330815 0.476251 11.00000 -1.50000 H44B 2 0.511237 1.235815 0.393303 11.00000 -1.50000 H44C 2 0.706133 1.296985 0.414317 11.00000 -1.50000 AFIX 0 MOLE 5 BR1 5 0.760660 0.622000 0.437389 11.00000 0.02891 0.01972 = 0.02674 0.00323 0.00477 0.00399 MOLE 6 O1W 4 0.045335 0.382046 0.386349 11.00000 0.03126 0.02460 = 0.03529 -0.00246 -0.00039 0.00761 H1W 2 -0.021798 0.446740 0.396053 11.00000 0.05623 H2W 2 0.099561 0.374486 0.426816 11.00000 0.06129 HKLF 4 Covalent radii and connectivity table for 04skc0008p-1 in P-1 C 0.770 H 0.320 N 0.700 O 0.660 BR 1.140 C1 - O1B O1A C2 C2 - O2 C1 C3 C3 - O3 C4 C2 C4 - O4A O4B C3 O1A - C1 O1B - C1 O2 - C2 O3 - C3 O4A - C4 O4B - C4 C22A - C23A N21 C22B - N21 C23B C22C - N21 C23C C22D - C23D N21 C23A - C22A C23B - C22B C23C - C22C C23D - C22D N21 - C22C C22B C22A C22D C31 - O31B O31A C32 C32 - O32 C33 C31 C33 - O33 C32 C34 C34 - O34A O34B C33 O31A - C31 O31B - C31 O32 - C32 O33 - C33 O34A - C34 O34B - C34 N41 - C43 C44 C42 C42 - N41 C42_$2 C43 - N41 C44 - N41 Br1 - no bonds found O1W - no bonds found Operators for generating equivalent atoms: $1 x, y+1, z+1 $2 -x+1, -y+2, -z+1 $3 -x, -y+1, -z+1 $4 x-1, y, z $5 x+1, y, z $6 -x+2, -y+1, -z $7 -x+1, -y+1, -z+1 28360 Reflections read, of which 124 rejected -10 =< h =< 10, -12 =< k =< 12, -23 =< l =< 22, Max. 2-theta = 54.97 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 3 -3 2 241.47 6.49 6 298.83 -3 -6 12 1.42 0.26 7 2.78 2 Inconsistent equivalents 6035 Unique reflections, of which 0 suppressed R(int) = 0.0616 R(sigma) = 0.0573 Friedel opposites merged Maximum memory for data reduction = 4124 / 60596 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 = 5124 / 426058 wR2 = 0.1123 before cycle 1 for 6035 data and 337 / 337 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. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.008 0.004 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.038; Restrained GooF = 1.038 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0498 * P )^2 + 1.26 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.57170 0.00086 -0.007 OSF Mean shift/esd = 0.009 Maximum = -0.051 for U22 Br1 Max. shift = 0.001 A for H33O Max. dU = 0.000 for H2W Least-squares cycle 2 Maximum vector length = 511 Memory required = 5124 / 426058 wR2 = 0.1123 before cycle 2 for 6035 data and 337 / 337 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. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.007 0.004 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.038; Restrained GooF = 1.038 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0498 * P )^2 + 1.26 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.57169 0.00086 -0.019 OSF Mean shift/esd = 0.003 Maximum = -0.019 for OSF Max. shift = 0.000 A for H4B Max. dU = 0.000 for H1W Least-squares cycle 3 Maximum vector length = 511 Memory required = 5124 / 426058 wR2 = 0.1123 before cycle 3 for 6035 data and 337 / 337 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. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.007 0.004 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.038; Restrained GooF = 1.038 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0498 * P )^2 + 1.26 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.57169 0.00086 -0.001 OSF Mean shift/esd = 0.000 Maximum = 0.004 for tors H4B Max. shift = 0.000 A for H4B Max. dU = 0.000 for H1W Least-squares cycle 4 Maximum vector length = 511 Memory required = 5124 / 426058 wR2 = 0.1123 before cycle 4 for 6035 data and 337 / 337 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. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.007 0.004 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.038; Restrained GooF = 1.038 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0498 * P )^2 + 1.26 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.57169 0.00086 -0.001 OSF Mean shift/esd = 0.000 Maximum = 0.001 for tors H4B Max. shift = 0.000 A for H4B Max. dU = 0.000 for H1W Largest correlation matrix elements 0.719 y H1W / x H1W 0.526 U22 Br1 / OSF 0.520 U33 Br1 / OSF Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2 0.1033 1.2056 0.7108 13 1.000 0.000 C2 O2 C1 C3 H3 0.0693 1.0114 0.7736 13 1.000 0.000 C3 O3 C4 C2 H1 0.4549 1.1597 0.8151 147 0.840 0.000 O1A C1 H1 H2O 0.1643 1.1611 0.5954 147 0.840 0.000 O2 C2 H2O H3O 0.0500 0.8044 0.6674 147 0.840 0.000 O3 C3 H3O H4B -0.3080 1.1018 0.7051 147 0.840 0.000 O4B C4 H4B H22A 0.3213 0.3351 0.2943 23 0.990 0.000 C22A C23A N21 H22B 0.5062 0.4172 0.3134 23 0.990 0.000 C22A C23A N21 H22C 0.3247 0.2817 0.0897 23 0.990 0.000 C22B N21 C23B H22D 0.2383 0.4107 0.1407 23 0.990 0.000 C22B N21 C23B H22E 0.4447 0.1400 0.2140 23 0.990 0.000 C22C N21 C23C H22F 0.6256 0.2261 0.2403 23 0.990 0.000 C22C N21 C23C H22G 0.5861 0.4093 0.1164 23 0.990 0.000 C22D C23D N21 H22H 0.5098 0.5380 0.1721 23 0.990 0.000 C22D C23D N21 H23A 0.4009 0.6186 0.2809 137 0.980 0.000 C23A C22A H23A H23B 0.2779 0.5692 0.3396 137 0.980 0.000 C23A C22A H23A H23C 0.2190 0.5369 0.2500 137 0.980 0.000 C23A C22A H23A H23D 0.1964 0.1237 0.1570 137 0.980 0.000 C23B C22B H23D H23E 0.0530 0.2071 0.1193 137 0.980 0.000 C23B C22B H23D H23F 0.1109 0.2528 0.2088 137 0.980 0.000 C23B C22B H23D H23G 0.5030 0.1162 0.0848 137 0.980 0.000 C23C C22C H23G H23H 0.6505 0.0508 0.1311 137 0.980 0.000 C23C C22C H23G H23I 0.6837 0.2033 0.1108 137 0.980 0.000 C23C C22C H23G H23J 0.7217 0.5221 0.2697 137 0.980 0.000 C23D C22D H23J H23K 0.8089 0.5469 0.1949 137 0.980 0.000 C23D C22D H23J H23L 0.7977 0.3922 0.2143 137 0.980 0.000 C23D C22D H23J H32 0.9406 0.1857 -0.1392 13 1.000 0.000 C32 O32 C33 C31 H33 0.8639 0.1523 -0.0200 13 1.000 0.000 C33 O33 C32 C34 H31A 1.3546 0.3481 -0.0520 147 0.840 0.000 O31A C31 H31A H32O 0.9807 0.4630 -0.0852 147 0.840 0.000 O32 C32 H32O H33O 0.8004 0.4076 0.0364 147 0.840 0.000 O33 C33 H33O H41 0.6738 1.0616 0.4217 13 0.930 0.000 N41 C43 C44 C42 H42A 0.3890 1.0715 0.4554 23 0.990 0.000 C42 N41 C42_$2 H42B 0.4658 1.1377 0.5413 23 0.990 0.000 C42 N41 C42_$2 H43A 0.7690 1.2268 0.5650 137 0.980 0.000 C43 N41 H43A H43B 0.8936 1.1979 0.4972 137 0.980 0.000 C43 N41 H43A H43C 0.8279 1.0702 0.5348 137 0.980 0.000 C43 N41 H43A H44A 0.5681 1.3308 0.4763 137 0.980 0.000 C44 N41 H44A H44B 0.5112 1.2358 0.3933 137 0.980 0.000 C44 N41 H44A H44C 0.7061 1.2970 0.4143 137 0.980 0.000 C44 N41 H44A 04skc0008p-1 in P-1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.34064 1.12243 0.72522 1.00000 0.01913 0.01350 0.01916 0.00014 0.00025 0.00151 0.01777 0.00506 0.00035 0.00026 0.00015 0.00000 0.00141 0.00124 0.00136 0.00100 0.00108 0.00105 0.00055 C2 0.15566 1.11413 0.69128 1.00000 0.01459 0.01763 0.01384 0.00050 -0.00070 0.00202 0.01580 0.00492 0.00033 0.00027 0.00014 0.00000 0.00131 0.00128 0.00124 0.00097 0.00099 0.00102 0.00052 H2 0.10328 1.20562 0.71077 1.00000 0.01896 0.00000 0.00000 C3 0.05587 0.99399 0.71647 1.00000 0.01549 0.01793 0.01703 0.00082 0.00068 0.00408 0.01714 0.00515 0.00034 0.00027 0.00015 0.00000 0.00133 0.00130 0.00129 0.00100 0.00103 0.00104 0.00053 H3 0.06929 1.01138 0.77365 1.00000 0.02057 0.00000 0.00000 C4 -0.13373 0.98947 0.69168 1.00000 0.01793 0.01847 0.01566 0.00451 0.00180 0.00396 0.01710 0.00523 0.00034 0.00028 0.00014 0.00000 0.00138 0.00132 0.00128 0.00103 0.00104 0.00108 0.00054 O1A 0.35493 1.16972 0.79747 1.00000 0.01556 0.03763 0.01730 -0.00470 -0.00294 0.00268 0.02513 0.00370 0.00025 0.00022 0.00010 0.00000 0.00101 0.00120 0.00099 0.00084 0.00077 0.00089 0.00045 H1 0.45488 1.15968 0.81513 1.00000 0.03770 0.00000 0.00000 O1B 0.45780 1.08514 0.68429 1.00000 0.01596 0.02732 0.01826 0.00090 0.00103 0.00405 0.02098 0.00363 0.00023 0.00020 0.00010 0.00000 0.00099 0.00104 0.00095 0.00077 0.00077 0.00081 0.00041 O2 0.14196 1.08592 0.61055 1.00000 0.02051 0.02064 0.01391 0.00325 -0.00149 0.00046 0.01856 0.00352 0.00024 0.00019 0.00010 0.00000 0.00100 0.00095 0.00090 0.00071 0.00074 0.00079 0.00039 H2O 0.16429 1.16108 0.59535 1.00000 0.02784 0.00000 0.00000 O3 0.12825 0.86560 0.68785 1.00000 0.01859 0.01526 0.03237 0.00089 -0.00202 0.00213 0.02280 0.00375 0.00025 0.00019 0.00011 0.00000 0.00102 0.00093 0.00113 0.00080 0.00085 0.00077 0.00042 H3O 0.04996 0.80437 0.66741 1.00000 0.03421 0.00000 0.00000 O4A -0.21199 0.88556 0.65397 1.00000 0.02053 0.02064 0.03548 0.00092 -0.00600 0.00043 0.02667 0.00381 0.00025 0.00020 0.00012 0.00000 0.00108 0.00103 0.00118 0.00087 0.00088 0.00084 0.00046 O4B -0.20194 1.11015 0.71758 1.00000 0.01356 0.02345 0.02757 -0.00425 -0.00001 0.00198 0.02292 0.00364 0.00024 0.00020 0.00011 0.00000 0.00097 0.00102 0.00106 0.00080 0.00082 0.00079 0.00043 H4B -0.30803 1.10182 0.70514 1.00000 0.03438 0.00000 0.00000 C22A 0.40019 0.40490 0.27841 1.00000 0.03559 0.02940 0.01868 0.00475 0.00681 0.00222 0.02769 0.00621 0.00042 0.00032 0.00016 0.00000 0.00177 0.00159 0.00144 0.00117 0.00125 0.00132 0.00066 H22A 0.32134 0.33508 0.29433 1.00000 0.03323 0.00000 0.00000 H22B 0.50615 0.41721 0.31337 1.00000 0.03323 0.00000 0.00000 C22B 0.28847 0.31868 0.14151 1.00000 0.02740 0.03657 0.02284 0.01187 -0.00419 0.00391 0.02837 0.00603 0.00040 0.00034 0.00017 0.00000 0.00166 0.00173 0.00152 0.00126 0.00123 0.00134 0.00067 H22C 0.32470 0.28166 0.08973 1.00000 0.03404 0.00000 0.00000 H22D 0.23828 0.41066 0.14072 1.00000 0.03404 0.00000 0.00000 C22C 0.52953 0.20742 0.19978 1.00000 0.02712 0.02305 0.03076 0.01064 0.00060 0.00639 0.02619 0.00612 0.00040 0.00030 0.00017 0.00000 0.00164 0.00148 0.00161 0.00121 0.00126 0.00124 0.00064 H22E 0.44471 0.13997 0.21402 1.00000 0.03143 0.00000 0.00000 H22F 0.62557 0.22607 0.24029 1.00000 0.03143 0.00000 0.00000 C22D 0.56659 0.44812 0.17044 1.00000 0.03462 0.02512 0.02095 0.00589 0.00843 -0.00224 0.02657 0.00590 0.00040 0.00031 0.00016 0.00000 0.00175 0.00152 0.00146 0.00115 0.00125 0.00129 0.00065 H22G 0.58611 0.40928 0.11638 1.00000 0.03188 0.00000 0.00000 H22H 0.50979 0.53805 0.17211 1.00000 0.03188 0.00000 0.00000 C23A 0.31724 0.54464 0.28807 1.00000 0.05588 0.03299 0.03529 0.00059 0.01996 0.01150 0.04122 0.00754 0.00051 0.00036 0.00020 0.00000 0.00238 0.00183 0.00187 0.00143 0.00168 0.00166 0.00086 H23A 0.40090 0.61863 0.28092 1.00000 0.06183 0.00000 0.00000 H23B 0.27788 0.56916 0.33960 1.00000 0.06183 0.00000 0.00000 H23C 0.21904 0.53691 0.24999 1.00000 0.06183 0.00000 0.00000 C23B 0.14994 0.21655 0.15812 1.00000 0.02542 0.06718 0.03828 0.02350 -0.00788 -0.00908 0.04274 0.00719 0.00044 0.00044 0.00021 0.00000 0.00179 0.00252 0.00196 0.00176 0.00145 0.00167 0.00089 H23D 0.19642 0.12372 0.15703 1.00000 0.06412 0.00000 0.00000 H23E 0.05300 0.20711 0.11926 1.00000 0.06412 0.00000 0.00000 H23F 0.11089 0.25281 0.20882 1.00000 0.06412 0.00000 0.00000 C23C 0.59773 0.13834 0.12504 1.00000 0.04467 0.02310 0.04438 0.00395 0.00989 0.00919 0.03728 0.00707 0.00048 0.00034 0.00020 0.00000 0.00210 0.00159 0.00201 0.00139 0.00160 0.00144 0.00079 H23G 0.50304 0.11618 0.08480 1.00000 0.05591 0.00000 0.00000 H23H 0.65054 0.05081 0.13112 1.00000 0.05591 0.00000 0.00000 H23I 0.68372 0.20334 0.11084 1.00000 0.05591 0.00000 0.00000 C23D 0.73892 0.48013 0.21640 1.00000 0.03886 0.03899 0.02873 0.00003 0.00354 -0.01804 0.03713 0.00609 0.00045 0.00037 0.00018 0.00000 0.00200 0.00189 0.00170 0.00138 0.00144 0.00153 0.00080 H23J 0.72172 0.52207 0.26973 1.00000 0.05569 0.00000 0.00000 H23K 0.80890 0.54686 0.19489 1.00000 0.05569 0.00000 0.00000 H23L 0.79770 0.39219 0.21435 1.00000 0.05569 0.00000 0.00000 N21 0.44592 0.34440 0.19773 1.00000 0.02304 0.02010 0.01599 0.00429 0.00087 0.00245 0.01963 0.00445 0.00030 0.00024 0.00012 0.00000 0.00127 0.00115 0.00111 0.00088 0.00092 0.00095 0.00048 C31 1.15218 0.25232 -0.06332 1.00000 0.01929 0.03201 0.01722 -0.00623 0.00193 0.00589 0.02427 0.00556 0.00037 0.00032 0.00015 0.00000 0.00149 0.00166 0.00138 0.00115 0.00111 0.00126 0.00063 C32 0.96857 0.26537 -0.09411 1.00000 0.01974 0.03317 0.01964 -0.00170 0.00010 0.00283 0.02522 0.00571 0.00037 0.00032 0.00016 0.00000 0.00150 0.00163 0.00143 0.00117 0.00114 0.00124 0.00063 H32 0.94061 0.18572 -0.13923 1.00000 0.03027 0.00000 0.00000 C33 0.84767 0.24604 -0.03421 1.00000 0.02161 0.02653 0.01927 -0.00334 -0.00223 0.00157 0.02379 0.00535 0.00037 0.00031 0.00016 0.00000 0.00150 0.00152 0.00141 0.00112 0.00114 0.00119 0.00061 H33 0.86390 0.15227 -0.01997 1.00000 0.02855 0.00000 0.00000 C34 0.66493 0.24828 -0.06808 1.00000 0.01852 0.02990 0.01863 -0.00042 -0.00094 -0.00073 0.02330 0.00540 0.00036 0.00031 0.00015 0.00000 0.00146 0.00156 0.00141 0.00116 0.00113 0.00121 0.00061 O31A 1.25175 0.36650 -0.05964 1.00000 0.01363 0.03111 0.02870 -0.00050 -0.00007 0.00546 0.02538 0.00385 0.00025 0.00021 0.00011 0.00000 0.00099 0.00113 0.00110 0.00086 0.00084 0.00085 0.00045 H31A 1.35460 0.34812 -0.05201 1.00000 0.03807 0.00000 0.00000 O31B 1.19638 0.14601 -0.04379 1.00000 0.02425 0.03041 0.03580 -0.00080 0.00453 0.00170 0.03112 0.00412 0.00027 0.00023 0.00012 0.00000 0.00115 0.00118 0.00123 0.00094 0.00094 0.00093 0.00049 O32 0.93942 0.39401 -0.11910 1.00000 0.02703 0.03084 0.02906 0.00731 -0.00282 0.00109 0.02909 0.00413 0.00028 0.00022 0.00012 0.00000 0.00118 0.00114 0.00116 0.00090 0.00090 0.00093 0.00047 H32O 0.98074 0.46302 -0.08519 1.00000 0.04364 0.00000 0.00000 O33 0.88287 0.35477 0.03175 1.00000 0.01805 0.02434 0.01443 -0.00366 -0.00028 0.00239 0.02006 0.00344 0.00024 0.00020 0.00010 0.00000 0.00100 0.00102 0.00092 0.00074 0.00075 0.00079 0.00040 H33O 0.80040 0.40764 0.03645 1.00000 0.03009 0.00000 0.00000 O34A 0.57336 0.33607 -0.03515 1.00000 0.01451 0.03190 0.02806 -0.00393 0.00018 0.00360 0.02625 0.00380 0.00024 0.00021 0.00011 0.00000 0.00100 0.00114 0.00110 0.00087 0.00083 0.00086 0.00046 O34B 0.62384 0.15236 -0.12819 1.00000 0.02513 0.03520 0.02544 -0.00059 -0.00193 -0.00015 0.02981 0.00394 0.00027 0.00023 0.00011 0.00000 0.00116 0.00121 0.00111 0.00090 0.00088 0.00093 0.00048 N41 0.64595 1.12944 0.46302 1.00000 0.01873 0.01675 0.01443 -0.00001 0.00247 -0.00037 0.01708 0.00418 0.00028 0.00023 0.00012 0.00000 0.00119 0.00110 0.00108 0.00084 0.00088 0.00090 0.00046 H41 0.67384 1.06160 0.42168 1.00000 0.02050 0.00000 0.00000 C42 0.48887 1.07368 0.49290 1.00000 0.02276 0.02162 0.02410 0.00578 0.00564 0.00110 0.02250 0.00575 0.00037 0.00029 0.00016 0.00000 0.00152 0.00144 0.00146 0.00113 0.00116 0.00115 0.00060 H42A 0.38899 1.07152 0.45539 1.00000 0.02700 0.00000 0.00000 H42B 0.46584 1.13765 0.54126 1.00000 0.02700 0.00000 0.00000 C43 0.79683 1.15854 0.51980 1.00000 0.02528 0.03793 0.02626 0.00448 -0.00565 -0.00295 0.03066 0.00589 0.00040 0.00035 0.00017 0.00000 0.00167 0.00177 0.00158 0.00131 0.00126 0.00136 0.00069 H43A 0.76896 1.22677 0.56503 1.00000 0.04599 0.00000 0.00000 H43B 0.89361 1.19789 0.49719 1.00000 0.04599 0.00000 0.00000 H43C 0.82788 1.07023 0.53478 1.00000 0.04599 0.00000 0.00000 C44 0.60427 1.25938 0.43426 1.00000 0.03058 0.02228 0.03406 0.01054 0.00672 0.00525 0.02799 0.00633 0.00041 0.00031 0.00018 0.00000 0.00170 0.00147 0.00169 0.00124 0.00133 0.00126 0.00066 H44A 0.56807 1.33082 0.47625 1.00000 0.04199 0.00000 0.00000 H44B 0.51121 1.23582 0.39332 1.00000 0.04199 0.00000 0.00000 H44C 0.70612 1.29696 0.41430 1.00000 0.04199 0.00000 0.00000 Br1 0.76066 0.62200 0.43739 1.00000 0.02891 0.01971 0.02673 0.00323 0.00477 0.00399 0.02513 0.00057 0.00004 0.00003 0.00002 0.00000 0.00018 0.00015 0.00017 0.00011 0.00012 0.00011 0.00010 O1W 0.04534 0.38205 0.38635 1.00000 0.03124 0.02460 0.03525 -0.00247 -0.00039 0.00760 0.03155 0.00434 0.00031 0.00023 0.00013 0.00000 0.00129 0.00116 0.00132 0.00094 0.00103 0.00098 0.00050 H1W -0.02179 0.44677 0.39608 1.00000 0.05608 0.07521 0.00428 0.00338 0.00203 0.00000 0.01277 H2W 0.09954 0.37452 0.42683 1.00000 0.06114 0.06943 0.00479 0.00427 0.00159 0.00000 0.01386 Final Structure Factor Calculation for 04skc0008p-1 in P-1 Total number of l.s. parameters = 337 Maximum vector length = 511 Memory required = 4787 / 24017 wR2 = 0.1123 before cycle 5 for 6035 data and 0 / 337 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. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.007 0.004 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.038; Restrained GooF = 1.038 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0498 * P )^2 + 1.26 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0456 for 4755 Fo > 4sig(Fo) and 0.0672 for all 6035 data wR2 = 0.1123, GooF = S = 1.038, Restrained GooF = 1.038 for all data Occupancy sum of asymmetric unit = 35.00 for non-hydrogen and 42.00 for hydrogen atoms Principal mean square atomic displacements U 0.0223 0.0185 0.0126 C1 0.0205 0.0146 0.0123 C2 0.0224 0.0159 0.0131 C3 0.0209 0.0158 0.0146 C4 0.0450 0.0184 0.0120 O1A 0.0302 0.0176 0.0151 O1B 0.0220 0.0207 0.0130 O2 0.0358 0.0178 0.0148 O3 0.0418 0.0213 0.0168 O4A 0.0379 0.0174 0.0134 O4B 0.0365 0.0296 0.0170 C22A 0.0377 0.0320 0.0154 C22B 0.0325 0.0298 0.0163 C22C 0.0383 0.0249 0.0164 C22D 0.0636 0.0408 0.0193 C23A 0.0753 0.0326 0.0203 C23B 0.0503 0.0414 0.0202 C23C 0.0629 0.0290 0.0194 C23D 0.0235 0.0197 0.0156 N21 0.0417 0.0192 0.0119 C31 0.0383 0.0198 0.0175 C32 0.0344 0.0224 0.0146 C33 0.0336 0.0210 0.0154 C34 0.0393 0.0243 0.0125 O31A 0.0433 0.0268 0.0233 O31B 0.0340 0.0303 0.0230 O32 0.0308 0.0178 0.0115 O33 0.0432 0.0214 0.0141 O34A 0.0405 0.0286 0.0203 O34B 0.0214 0.0172 0.0127 N41 0.0269 0.0219 0.0186 C42 0.0400 0.0337 0.0183 C43 0.0374 0.0275 0.0190 C44 0.0303 0.0264 0.0186 Br1 0.0455 0.0298 0.0193 O1W Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.020 0.033 0.048 0.065 0.081 0.099 0.119 0.150 0.206 1.000 Number in group 635. 589. 592. 626. 582. 619. 589. 596. 603. 604. GooF 0.928 0.978 1.032 1.124 1.048 1.142 1.011 1.031 0.973 1.089 K 1.433 1.031 0.973 0.980 0.976 0.986 0.996 1.005 1.017 1.002 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.05 1.15 1.32 1.64 inf Number in group 603. 612. 604. 601. 596. 611. 603. 600. 598. 607. GooF 1.003 0.913 0.972 0.951 0.928 0.945 0.954 0.928 1.111 1.523 K 0.988 1.008 1.010 0.994 1.001 1.008 1.020 1.028 1.028 0.981 R1 0.182 0.132 0.119 0.097 0.068 0.053 0.043 0.034 0.035 0.036 Recommended weighting scheme: WGHT 0.0496 1.2652 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 1 0 1209.70 2115.51 5.62 0.263 6.20 -2 -1 6 369.24 236.07 5.22 0.088 2.43 0 -4 3 34.30 4.08 4.78 0.012 2.36 -1 -1 5 441.82 301.60 4.69 0.099 3.28 2 -2 1 331.78 486.27 4.58 0.126 3.09 -1 2 1 368.27 254.73 4.44 0.091 3.92 1 -4 2 42.90 95.29 4.42 0.056 2.33 -3 -1 5 371.79 260.31 4.15 0.092 2.15 2 -1 3 188.17 282.31 4.13 0.096 3.12 -1 -2 2 748.90 996.42 4.12 0.180 3.91 1 -3 2 763.32 581.07 3.94 0.138 2.98 -3 3 7 62.50 23.50 3.92 0.028 1.54 -3 -1 4 297.22 207.77 3.91 0.082 2.28 1 -4 1 114.95 66.16 3.82 0.046 2.33 -2 0 8 344.23 471.47 3.76 0.124 1.98 2 -5 5 57.45 109.60 3.74 0.060 1.66 -4 -2 16 -5.18 26.37 3.72 0.029 1.00 2 1 2 327.41 443.54 3.68 0.120 3.11 1 -1 5 334.45 246.51 3.58 0.090 3.14 -2 5 0 142.86 88.51 3.54 0.054 1.74 2 3 0 237.37 168.81 3.46 0.074 2.38 1 -5 2 140.36 206.23 3.43 0.082 1.89 4 2 8 145.43 215.87 3.41 0.084 1.28 -5 6 15 89.72 184.82 3.36 0.078 0.78 -1 3 7 232.60 166.85 3.34 0.074 1.78 0 -2 2 6427.15 8153.08 3.30 0.516 4.56 0 -4 4 185.55 126.14 3.30 0.064 2.28 -4 -2 6 761.30 597.59 3.29 0.140 1.62 -3 -4 1 93.54 54.63 3.27 0.042 1.72 -9 -1 3 122.07 249.55 3.24 0.090 0.86 -1 -8 9 10.39 44.72 3.23 0.038 1.10 -1 12 1 60.77 156.00 3.23 0.071 0.78 -4 -5 1 164.94 235.53 3.17 0.088 1.33 9 -1 3 65.77 164.71 3.13 0.073 0.85 -3 2 5 215.18 153.64 3.11 0.071 1.92 -6 -5 9 153.56 238.78 3.11 0.088 0.99 3 -1 4 214.81 156.37 3.07 0.071 2.18 0 -11 12 152.63 252.90 3.06 0.091 0.82 -2 -7 5 42.91 5.37 3.05 0.013 1.27 0 2 2 1716.08 2060.00 3.04 0.259 3.83 -3 -6 18 180.90 265.72 3.04 0.093 0.87 -8 -5 3 238.47 95.23 3.03 0.056 0.86 2 -10 2 151.00 253.65 3.03 0.091 0.94 -4 -4 19 34.63 85.41 3.01 0.053 0.85 3 -4 5 613.33 493.68 3.01 0.127 1.67 -2 -8 10 1414.68 1144.78 2.99 0.193 1.05 1 -7 18 203.87 292.61 2.98 0.098 0.87 -2 -5 6 1173.14 1459.04 2.98 0.218 1.60 -3 3 2 3235.58 2743.28 2.97 0.299 1.98 -5 0 1 154.09 101.64 2.96 0.058 1.56 Bond lengths and angles C1 - Distance Angles O1B 1.2358 (0.0032) O1A 1.2763 (0.0031) 126.76 (0.25) C2 1.5218 (0.0037) 120.92 (0.23) 112.32 (0.22) C1 - O1B O1A C2 - Distance Angles O2 1.4104 (0.0030) C1 1.5218 (0.0037) 112.62 (0.21) C3 1.5281 (0.0037) 107.77 (0.20) 108.71 (0.20) H2 1.0000 109.23 109.23 109.23 C2 - O2 C1 C3 C3 - Distance Angles O3 1.4039 (0.0031) C4 1.5143 (0.0037) 111.99 (0.21) C2 1.5281 (0.0037) 108.94 (0.21) 111.56 (0.21) H3 1.0000 108.07 108.07 108.07 C3 - O3 C4 C2 C4 - Distance Angles O4A 1.2032 (0.0033) O4B 1.3164 (0.0031) 124.60 (0.25) C3 1.5143 (0.0037) 123.09 (0.24) 112.29 (0.22) C4 - O4A O4B O1A - Distance Angles C1 1.2763 (0.0031) H1 0.8400 109.47 O1A - C1 O1B - Distance Angles C1 1.2358 (0.0032) O1B - O2 - Distance Angles C2 1.4104 (0.0030) H2O 0.8400 109.47 O2 - C2 O3 - Distance Angles C3 1.4039 (0.0031) H3O 0.8400 109.47 O3 - C3 O4A - Distance Angles C4 1.2032 (0.0033) O4A - O4B - Distance Angles C4 1.3164 (0.0031) H4B 0.8400 109.47 O4B - C4 C22A - Distance Angles C23A 1.5086 (0.0044) N21 1.5188 (0.0035) 115.00 (0.24) H22A 0.9900 108.52 108.52 H22B 0.9900 108.52 108.52 107.52 C22A - C23A N21 H22A C22B - Distance Angles N21 1.5121 (0.0037) C23B 1.5166 (0.0045) 115.17 (0.24) H22C 0.9900 108.48 108.48 H22D 0.9900 108.48 108.48 107.50 C22B - N21 C23B H22C C22C - Distance Angles N21 1.5087 (0.0035) C23C 1.5146 (0.0044) 114.43 (0.23) H22E 0.9900 108.65 108.65 H22F 0.9900 108.65 108.65 107.59 C22C - N21 C23C H22E C22D - Distance Angles C23D 1.5137 (0.0046) N21 1.5190 (0.0036) 114.69 (0.24) H22G 0.9900 108.59 108.59 H22H 0.9900 108.59 108.59 107.56 C22D - C23D N21 H22G C23A - Distance Angles C22A 1.5086 (0.0044) H23A 0.9800 109.47 H23B 0.9800 109.47 109.47 H23C 0.9800 109.47 109.47 109.47 C23A - C22A H23A H23B C23B - Distance Angles C22B 1.5166 (0.0045) H23D 0.9800 109.47 H23E 0.9800 109.47 109.47 H23F 0.9800 109.47 109.47 109.47 C23B - C22B H23D H23E C23C - Distance Angles C22C 1.5146 (0.0044) H23G 0.9800 109.47 H23H 0.9800 109.47 109.47 H23I 0.9800 109.47 109.47 109.47 C23C - C22C H23G H23H C23D - Distance Angles C22D 1.5137 (0.0046) H23J 0.9800 109.47 H23K 0.9800 109.47 109.47 H23L 0.9800 109.47 109.47 109.47 C23D - C22D H23J H23K N21 - Distance Angles C22C 1.5087 (0.0035) C22B 1.5121 (0.0037) 110.53 (0.22) C22A 1.5188 (0.0035) 107.25 (0.21) 111.33 (0.23) C22D 1.5190 (0.0036) 110.80 (0.22) 106.41 (0.21) 110.58 (0.22) N21 - C22C C22B C22A C31 - Distance Angles O31B 1.2067 (0.0036) O31A 1.3076 (0.0036) 124.97 (0.27) C32 1.5221 (0.0040) 121.66 (0.28) 113.37 (0.25) C31 - O31B O31A C32 - Distance Angles O32 1.4250 (0.0036) C33 1.5126 (0.0040) 110.09 (0.23) C31 1.5221 (0.0040) 114.82 (0.25) 109.35 (0.23) H32 1.0000 107.43 107.43 107.43 C32 - O32 C33 C31 C33 - Distance Angles O33 1.4135 (0.0032) C32 1.5126 (0.0040) 110.07 (0.23) C34 1.5160 (0.0040) 110.82 (0.23) 108.53 (0.23) H33 1.0000 109.13 109.13 109.13 C33 - O33 C32 C34 C34 - Distance Angles O34A 1.2227 (0.0034) O34B 1.2804 (0.0034) 127.56 (0.27) C33 1.5160 (0.0040) 118.12 (0.24) 114.29 (0.24) C34 - O34A O34B O31A - Distance Angles C31 1.3076 (0.0036) H31A 0.8400 109.47 O31A - C31 O31B - Distance Angles C31 1.2067 (0.0036) O31B - O32 - Distance Angles C32 1.4250 (0.0036) H32O 0.8400 109.47 O32 - C32 O33 - Distance Angles C33 1.4135 (0.0032) H33O 0.8400 109.47 O33 - C33 O34A - Distance Angles C34 1.2227 (0.0034) O34A - O34B - Distance Angles C34 1.2804 (0.0034) O34B - N41 - Distance Angles C43 1.4794 (0.0036) C44 1.4901 (0.0034) 110.77 (0.23) C42 1.4948 (0.0035) 113.72 (0.22) 108.57 (0.21) H41 0.9300 107.86 107.86 107.86 N41 - C43 C44 C42 C42 - Distance Angles N41 1.4948 (0.0034) C42_$2 1.5107 (0.0053) 110.93 (0.29) H42A 0.9900 109.45 109.45 H42B 0.9900 109.45 109.45 108.04 C42 - N41 C42_$2 H42A C43 - Distance Angles N41 1.4794 (0.0036) H43A 0.9800 109.47 H43B 0.9800 109.47 109.47 H43C 0.9800 109.47 109.47 109.47 C43 - N41 H43A H43B C44 - Distance Angles N41 1.4901 (0.0034) H44A 0.9800 109.47 H44B 0.9800 109.47 109.47 H44C 0.9800 109.47 109.47 109.47 C44 - N41 H44A H44B O1W - Distance Angles H1W 0.8347 (0.0179) H2W 0.8310 (0.0178) 108.78 (2.68) O1W - H1W Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.84 2.24 2.713(3) 115.5 O3-H3O...O4A 0.84 2.12 2.606(3) 116.9 O33-H33O...O34A 0.84 1.62 2.440(3) 163.9 O1A-H1...O34B_$1 0.84 2.35 3.1839(19) 175.3 O2-H2O...Br1_$2 0.93 2.10 2.888(3) 141.5 N41-H41...O2_$2 0.93 2.27 3.039(3) 139.3 N41-H41...O1B_$2 0.84 1.95 2.736(3) 155.7 O3-H3O...O1W_$3 0.84 1.84 2.676(3) 176.4 O4B-H4B...O1B_$4 0.835(18) 2.501(19) 3.330(2) 172(4) O1W-H1W...Br1_$4 0.84 1.73 2.565(3) 171.7 O31A-H31A...O34A_$5 0.84 2.04 2.847(3) 161.9 O32-H32O...O33_$6 0.84 2.20 2.898(3) 140.7 O33-H33O...O31A_$6 0.831(18) 2.59(2) 3.410(2) 172(3) O1W-H2W...Br1_$7 FMAP and GRID set by program FMAP 2 1 37 GRID -2.941 -2 -1 2.941 2 1 R1 = 0.0642 for 6035 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 1.34 at 0.3552 0.7307 0.1497 [ 1.27 A from O34B ] Deepest hole -0.52 at 0.8606 0.6621 0.4614 [ 0.90 A from BR1 ] Mean = 0.00, Rms deviation from mean = 0.09 e/A^3, Highest memory used = 4737 / 42106 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.6448 0.2693 -0.1497 1.00000 0.05 1.34 1.27 O34B 1.51 C34 1.78 H1 2.14 O34A Q2 1 0.8822 0.0697 -0.0786 1.00000 0.05 1.01 1.21 H33 1.77 C33 1.78 H32 2.05 C32 Q3 1 0.8764 0.3341 -0.0513 1.00000 0.05 0.82 0.98 C33 1.21 C32 1.46 O33 1.55 O32 Q4 1 0.9616 0.1799 -0.0854 1.00000 0.05 0.57 0.87 C32 0.98 H32 1.41 C33 1.50 H33 Q5 1 0.6562 0.3382 -0.0759 1.00000 0.05 0.47 0.91 C34 1.01 O34A 1.85 O34B 1.96 C33 Q6 1 0.8604 0.4597 0.2728 1.00000 0.05 0.33 1.18 H23L 1.27 H23J 1.39 C23D 1.80 H23K Q7 1 0.0748 0.2853 0.1758 1.00000 0.05 0.32 0.77 H23F 0.93 C23B 1.13 H23E 1.85 H23D Q8 1 0.0532 0.3761 0.5114 1.00000 0.05 0.31 1.58 H2W 1.66 BR1 2.04 H43B 2.16 H1W Q9 1 0.1002 0.3098 0.4980 1.00000 0.05 0.31 1.53 H2W 1.55 BR1 1.90 H43B 2.27 O1W Q10 1 0.3795 0.1605 0.2713 1.00000 0.05 0.29 1.16 H22E 1.74 H22A 1.90 C22C 2.03 O4A Shortest distances between peaks (including symmetry equivalents) 8 9 0.76 2 4 1.24 1 5 1.35 3 4 1.68 3 5 1.75 1 3 2.40 2 3 2.50 8 8 2.67 6 7 2.86 4 5 2.89 1 4 2.90 Time profile in seconds ----------------------- 0.05: Read and process instructions 0.00: Fit rigid groups 0.02: 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. 1.30: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.00: Set up l.s. refinement 0.00: Generate idealized H-atoms 1.66: Structure factors and derivatives 4.31: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.05: Apply other restraints 0.33: Solve l.s. equations 0.00: Generate HTAB table 0.06: Other dependent quantities, CIF, tables 0.09: Analysis of variance 0.05: Merge reflections for Fourier and .fcf 0.13: Fourier summations 0.00: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 04skc0008p-1 finished at 11:17:39 Total CPU time: 8.0 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++