+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + shelxl started at 13:32:49 on 31-Mar-2009 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2009lsh001 in P2(1)/n CELL 0.71073 8.0497 17.7203 10.1483 90.000 102.323 90.000 ZERR 4.00 0.0002 0.0003 0.0003 0.000 0.002 0.000 LATT 1 SYMM 1/2 - X, 1/2 + Y, 1/2 - Z SFAC C H N O UNIT 60 72 8 8 V = 1414.23 F(000) = 552.0 Mu = 0.08 mm-1 Cell Wt = 1033.26 Rho = 1.213 MERG 2 OMIT -3.00 55.00 OMIT 0 4 1 OMIT -1 3 4 OMIT 0 10 0 OMIT 0 7 1 FMAP 2 PLAN 5 SIZE 0.60 0.60 0.90 ACTA BOND $H L.S. 6 TEMP -153.00 WGHT 0.042100 0.534300 FVAR 0.96143 C1 1 0.688584 0.140130 0.697151 11.00000 0.01657 0.01158 = 0.01316 0.00033 0.00342 0.00065 C2 1 0.833933 0.176103 0.770610 11.00000 0.01555 0.01371 = 0.01500 0.00186 0.00449 -0.00096 C3 1 0.821395 0.225876 0.874802 11.00000 0.02334 0.01488 = 0.01578 -0.00065 0.00302 -0.00466 AFIX 43 H3 2 0.920146 0.249945 0.925296 11.00000 -1.20000 AFIX 0 C4 1 0.663542 0.239840 0.903871 11.00000 0.03039 0.01456 = 0.01777 -0.00179 0.00867 0.00137 AFIX 43 H4 2 0.654062 0.273506 0.974747 11.00000 -1.20000 AFIX 0 C5 1 0.518979 0.204693 0.829547 11.00000 0.02107 0.01694 = 0.02334 0.00125 0.01056 0.00406 AFIX 43 H5 2 0.411173 0.214732 0.849722 11.00000 -1.20000 AFIX 0 C6 1 0.531119 0.154823 0.725626 11.00000 0.01526 0.01523 = 0.02108 0.00046 0.00405 -0.00019 AFIX 43 H6 2 0.432042 0.131142 0.674818 11.00000 -1.20000 AFIX 0 C7 1 0.707791 0.009401 0.618722 11.00000 0.02360 0.01527 = 0.01789 -0.00101 0.00435 0.00004 C8 1 0.729674 -0.012691 0.765437 11.00000 0.02636 0.01447 = 0.01686 -0.00031 0.00467 0.00083 AFIX 23 H8A 2 0.630865 0.005589 0.800039 11.00000 -1.20000 H8B 2 0.833019 0.011807 0.818614 11.00000 -1.20000 AFIX 0 C9 1 0.745025 -0.097853 0.783945 11.00000 0.03203 0.01435 = 0.02308 0.00064 0.00509 0.00245 AFIX 23 H9A 2 0.843223 -0.116035 0.748436 11.00000 -1.20000 H9B 2 0.641333 -0.122180 0.730958 11.00000 -1.20000 AFIX 0 C10 1 0.768376 -0.121214 0.931221 11.00000 0.05760 0.01817 = 0.02827 0.00702 0.00627 0.00231 AFIX 137 H10A 2 0.871135 -0.097426 0.984099 11.00000 -1.50000 H10B 2 0.779603 -0.176210 0.938405 11.00000 -1.50000 H10C 2 0.669411 -0.105035 0.965905 11.00000 -1.50000 AFIX 0 C11 1 0.712298 0.120852 0.465944 11.00000 0.01417 0.01774 = 0.01517 0.00005 0.00200 0.00060 C12 1 0.738039 0.071362 0.351314 11.00000 0.02542 0.01841 = 0.01582 -0.00180 0.00555 0.00145 AFIX 23 H12A 2 0.643037 0.034857 0.329443 11.00000 -1.20000 H12B 2 0.844646 0.042318 0.380303 11.00000 -1.20000 AFIX 0 C13 1 0.747258 0.116205 0.225182 11.00000 0.03636 0.02144 = 0.01877 -0.00093 0.01104 -0.00138 AFIX 23 H13A 2 0.848836 0.149197 0.243659 11.00000 -1.20000 H13B 2 0.645337 0.148666 0.199818 11.00000 -1.20000 AFIX 0 C14 1 0.757008 0.062894 0.109149 11.00000 0.05263 0.02709 = 0.01978 -0.00192 0.01564 -0.00111 AFIX 137 H14A 2 0.654523 0.031473 0.089006 11.00000 -1.50000 H14B 2 0.857478 0.030549 0.134737 11.00000 -1.50000 H14C 2 0.765289 0.092395 0.029122 11.00000 -1.50000 AFIX 0 C15 1 0.994677 0.160635 0.735874 11.00000 0.01772 0.02442 = 0.01701 -0.00181 0.00206 -0.00414 N1 3 0.704466 0.087565 0.591643 11.00000 0.01673 0.01335 = 0.01366 -0.00188 0.00360 0.00028 N2 3 1.120184 0.146766 0.704928 11.00000 0.01846 0.05065 = 0.03257 -0.00557 0.00816 -0.00196 O1 4 0.695198 -0.037436 0.530287 11.00000 0.06775 0.01592 = 0.02035 -0.00388 0.01205 -0.00215 O2 4 0.701280 0.189054 0.456306 11.00000 0.03183 0.01582 = 0.01930 0.00087 0.00658 0.00308 HKLF 4 Covalent radii and connectivity table for 2009lsh001 in P2(1)/n C 0.770 H 0.320 N 0.700 O 0.660 C1 - C6 C2 N1 C2 - C3 C1 C15 C3 - C4 C2 C4 - C3 C5 C5 - C4 C6 C6 - C1 C5 C7 - O1 N1 C8 C8 - C7 C9 C9 - C8 C10 C10 - C9 C11 - O2 N1 C12 C12 - C11 C13 C13 - C12 C14 C14 - C13 C15 - N2 C2 N1 - C7 C11 C1 N2 - C15 O1 - C7 O2 - C11 h k l Fo^2 Sigma Why rejected -2 0 1 17.44 4.34 observed but should be systematically absent -2 0 1 27.21 5.04 observed but should be systematically absent -2 0 3 6.67 1.58 observed but should be systematically absent -1 0 4 4.80 0.81 observed but should be systematically absent 18229 Reflections read, of which 329 rejected -10 =< h =< 10, -22 =< k =< 23, -13 =< l =< 13, Max. 2-theta = 54.99 4 Systematic absence violations 0 Inconsistent equivalents 3234 Unique reflections, of which 0 suppressed R(int) = 0.0359 R(sigma) = 0.0261 Friedel opposites merged Maximum memory for data reduction = 1924 / 32223 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 = 2422 / 216396 wR2 = 0.0987 before cycle 1 for 3234 data and 174 / 174 parameters GooF = S = 1.034; Restrained GooF = 1.034 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0421 * P )^2 + 0.53 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.96212 0.00175 0.397 OSF Mean shift/esd = 0.069 Maximum = 0.583 for y O1 Max. shift = 0.002 A for H10C Max. dU = 0.000 for C10 Least-squares cycle 2 Maximum vector length = 511 Memory required = 2422 / 216396 wR2 = 0.0986 before cycle 2 for 3234 data and 174 / 174 parameters GooF = S = 1.033; Restrained GooF = 1.033 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0421 * P )^2 + 0.53 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.96228 0.00175 0.091 OSF Mean shift/esd = 0.025 Maximum = 0.210 for y O1 Max. shift = 0.001 A for H10C Max. dU = 0.000 for C10 Least-squares cycle 3 Maximum vector length = 511 Memory required = 2422 / 216396 wR2 = 0.0986 before cycle 3 for 3234 data and 174 / 174 parameters GooF = S = 1.033; Restrained GooF = 1.033 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0421 * P )^2 + 0.53 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.96229 0.00175 0.005 OSF Mean shift/esd = 0.001 Maximum = -0.007 for U23 C11 Max. shift = 0.000 A for H14A Max. dU = 0.000 for C10 Least-squares cycle 4 Maximum vector length = 511 Memory required = 2422 / 216396 wR2 = 0.0986 before cycle 4 for 3234 data and 174 / 174 parameters GooF = S = 1.033; Restrained GooF = 1.033 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0421 * P )^2 + 0.53 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.96229 0.00175 0.001 OSF Mean shift/esd = 0.000 Maximum = 0.002 for U22 C11 Max. shift = 0.000 A for H14C Max. dU = 0.000 for C3 Least-squares cycle 5 Maximum vector length = 511 Memory required = 2422 / 216396 wR2 = 0.0986 before cycle 5 for 3234 data and 174 / 174 parameters GooF = S = 1.033; Restrained GooF = 1.033 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0421 * P )^2 + 0.53 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.96229 0.00175 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H4 Max. dU = 0.000 for C12 Least-squares cycle 6 Maximum vector length = 511 Memory required = 2422 / 216396 wR2 = 0.0986 before cycle 6 for 3234 data and 174 / 174 parameters GooF = S = 1.033; Restrained GooF = 1.033 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0421 * P )^2 + 0.53 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.96229 0.00175 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for z C1 Max. shift = 0.000 A for H14B Max. dU = 0.000 for C8 No correlation matrix elements larger than 0.500 Idealized hydrogen atom generation before cycle 7 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H3 0.9201 0.2499 0.9253 43 0.950 0.000 C3 C4 C2 H4 0.6541 0.2735 0.9748 43 0.950 0.000 C4 C3 C5 H5 0.4112 0.2148 0.8497 43 0.950 0.000 C5 C4 C6 H6 0.4320 0.1311 0.6748 43 0.950 0.000 C6 C1 C5 H8A 0.6309 0.0056 0.8000 23 0.990 0.000 C8 C7 C9 H8B 0.8330 0.0118 0.8186 23 0.990 0.000 C8 C7 C9 H9A 0.8432 -0.1160 0.7484 23 0.990 0.000 C9 C8 C10 H9B 0.6413 -0.1222 0.7310 23 0.990 0.000 C9 C8 C10 H10A 0.8713 -0.0975 0.9840 137 0.980 0.000 C10 C9 H10A H10B 0.7793 -0.1762 0.9384 137 0.980 0.000 C10 C9 H10A H10C 0.6695 -0.1049 0.9660 137 0.980 0.000 C10 C9 H10A H12A 0.6430 0.0349 0.3294 23 0.990 0.000 C12 C11 C13 H12B 0.8446 0.0423 0.3803 23 0.990 0.000 C12 C11 C13 H13A 0.8488 0.1492 0.2437 23 0.990 0.000 C13 C12 C14 H13B 0.6454 0.1487 0.1998 23 0.990 0.000 C13 C12 C14 H14A 0.6544 0.0315 0.0889 137 0.980 0.000 C14 C13 H14A H14B 0.8574 0.0305 0.1347 137 0.980 0.000 C14 C13 H14A H14C 0.7654 0.0924 0.0292 137 0.980 0.000 C14 C13 H14A 2009lsh001 in P2(1)/n ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.68858 0.14013 0.69714 1.00000 0.01664 0.01160 0.01320 0.00035 0.00342 0.00065 0.01378 0.00193 0.00013 0.00006 0.00010 0.00000 0.00053 0.00047 0.00047 0.00036 0.00039 0.00037 0.00022 C2 0.83393 0.17611 0.77061 1.00000 0.01560 0.01376 0.01504 0.00192 0.00451 -0.00095 0.01462 0.00197 0.00013 0.00006 0.00010 0.00000 0.00052 0.00048 0.00048 0.00038 0.00040 0.00039 0.00022 C3 0.82140 0.22586 0.87481 1.00000 0.02342 0.01483 0.01585 -0.00066 0.00303 -0.00466 0.01820 0.00205 0.00015 0.00006 0.00011 0.00000 0.00058 0.00051 0.00049 0.00039 0.00042 0.00042 0.00023 H3 0.92015 0.24992 0.92532 1.00000 0.02185 0.00000 0.00000 C4 0.66354 0.23981 0.90387 1.00000 0.03050 0.01452 0.01782 -0.00182 0.00869 0.00137 0.02042 0.00217 0.00015 0.00006 0.00011 0.00000 0.00065 0.00050 0.00052 0.00040 0.00045 0.00044 0.00024 H4 0.65408 0.27346 0.97478 1.00000 0.02450 0.00000 0.00000 C5 0.51899 0.20470 0.82956 1.00000 0.02115 0.01689 0.02340 0.00127 0.01059 0.00407 0.01961 0.00224 0.00015 0.00006 0.00011 0.00000 0.00057 0.00052 0.00055 0.00042 0.00045 0.00041 0.00024 H5 0.41119 0.21476 0.84974 1.00000 0.02353 0.00000 0.00000 C6 0.53111 0.15482 0.72561 1.00000 0.01532 0.01526 0.02112 0.00048 0.00405 -0.00019 0.01721 0.00207 0.00014 0.00006 0.00011 0.00000 0.00052 0.00051 0.00053 0.00040 0.00042 0.00039 0.00023 H6 0.43203 0.13114 0.67480 1.00000 0.02065 0.00000 0.00000 C7 0.70779 0.00939 0.61871 1.00000 0.02368 0.01519 0.01797 -0.00099 0.00437 0.00004 0.01896 0.00211 0.00015 0.00006 0.00011 0.00000 0.00058 0.00052 0.00053 0.00040 0.00044 0.00042 0.00024 C8 0.72967 -0.01269 0.76542 1.00000 0.02639 0.01454 0.01690 -0.00034 0.00468 0.00083 0.01927 0.00215 0.00015 0.00006 0.00011 0.00000 0.00059 0.00052 0.00052 0.00040 0.00043 0.00042 0.00024 H8A 0.63086 0.00559 0.80001 1.00000 0.02312 0.00000 0.00000 H8B 0.83301 0.01181 0.81859 1.00000 0.02312 0.00000 0.00000 C9 0.74503 -0.09784 0.78395 1.00000 0.03208 0.01439 0.02311 0.00068 0.00510 0.00246 0.02331 0.00231 0.00017 0.00006 0.00012 0.00000 0.00068 0.00054 0.00058 0.00042 0.00049 0.00045 0.00026 H9A 0.84323 -0.11603 0.74845 1.00000 0.02797 0.00000 0.00000 H9B 0.64134 -0.12218 0.73097 1.00000 0.02797 0.00000 0.00000 C10 0.76837 -0.12117 0.93122 1.00000 0.05761 0.01834 0.02829 0.00708 0.00627 0.00232 0.03518 0.00284 0.00021 0.00007 0.00014 0.00000 0.00095 0.00060 0.00067 0.00050 0.00062 0.00058 0.00033 H10A 0.87129 -0.09748 0.98404 1.00000 0.05277 0.00000 0.00000 H10B 0.77930 -0.17617 0.93842 1.00000 0.05277 0.00000 0.00000 H10C 0.66954 -0.10486 0.96596 1.00000 0.05277 0.00000 0.00000 C11 0.71230 0.12088 0.46595 1.00000 0.01424 0.01766 0.01523 0.00005 0.00202 0.00061 0.01588 0.00199 0.00013 0.00006 0.00010 0.00000 0.00051 0.00052 0.00050 0.00039 0.00039 0.00039 0.00022 C12 0.73803 0.07135 0.35130 1.00000 0.02542 0.01858 0.01584 -0.00180 0.00556 0.00144 0.01977 0.00215 0.00015 0.00006 0.00011 0.00000 0.00060 0.00054 0.00052 0.00041 0.00044 0.00044 0.00024 H12A 0.64302 0.03485 0.32943 1.00000 0.02373 0.00000 0.00000 H12B 0.84463 0.04230 0.38029 1.00000 0.02373 0.00000 0.00000 C13 0.74726 0.11620 0.22520 1.00000 0.03640 0.02149 0.01881 -0.00087 0.01104 -0.00137 0.02480 0.00237 0.00017 0.00007 0.00012 0.00000 0.00072 0.00058 0.00056 0.00044 0.00050 0.00049 0.00027 H13A 0.84885 0.14919 0.24369 1.00000 0.02976 0.00000 0.00000 H13B 0.64535 0.14867 0.19985 1.00000 0.02976 0.00000 0.00000 C14 0.75700 0.06292 0.10914 1.00000 0.05275 0.02692 0.01987 -0.00193 0.01566 -0.00112 0.03200 0.00268 0.00020 0.00008 0.00013 0.00000 0.00089 0.00065 0.00058 0.00049 0.00057 0.00058 0.00031 H14A 0.65444 0.03155 0.08889 1.00000 0.04799 0.00000 0.00000 H14B 0.85738 0.03052 0.13475 1.00000 0.04799 0.00000 0.00000 H14C 0.76545 0.09243 0.02917 1.00000 0.04799 0.00000 0.00000 C15 0.99468 0.16063 0.73586 1.00000 0.01776 0.02444 0.01706 -0.00176 0.00207 -0.00413 0.02000 0.00204 0.00015 0.00006 0.00011 0.00000 0.00057 0.00058 0.00051 0.00042 0.00043 0.00043 0.00024 N1 0.70447 0.08758 0.59165 1.00000 0.01674 0.01348 0.01370 -0.00189 0.00361 0.00027 0.01459 0.00165 0.00011 0.00005 0.00009 0.00000 0.00045 0.00043 0.00042 0.00033 0.00034 0.00033 0.00020 N2 1.12018 0.14676 0.70491 1.00000 0.01853 0.05057 0.03264 -0.00553 0.00818 -0.00194 0.03351 0.00219 0.00014 0.00007 0.00012 0.00000 0.00056 0.00074 0.00061 0.00052 0.00046 0.00048 0.00028 O1 0.69520 -0.03740 0.53028 1.00000 0.06782 0.01598 0.02041 -0.00389 0.01207 -0.00214 0.03434 0.00180 0.00014 0.00005 0.00009 0.00000 0.00073 0.00043 0.00044 0.00033 0.00044 0.00041 0.00025 O2 0.70128 0.18902 0.45630 1.00000 0.03184 0.01597 0.01932 0.00085 0.00659 0.00307 0.02221 0.00157 0.00011 0.00004 0.00008 0.00000 0.00048 0.00040 0.00040 0.00030 0.00034 0.00033 0.00019 Final Structure Factor Calculation for 2009lsh001 in P2(1)/n Total number of l.s. parameters = 174 Maximum vector length = 511 Memory required = 2248 / 22995 wR2 = 0.0986 before cycle 7 for 3234 data and 0 / 174 parameters GooF = S = 1.033; Restrained GooF = 1.033 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0421 * P )^2 + 0.53 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0401 for 2797 Fo > 4sig(Fo) and 0.0479 for all 3234 data wR2 = 0.0986, GooF = S = 1.033, Restrained GooF = 1.033 for all data Occupancy sum of asymmetric unit = 19.00 for non-hydrogen and 18.00 for hydrogen atoms Principal mean square atomic displacements U 0.0167 0.0131 0.0115 C1 0.0165 0.0159 0.0114 C2 0.0259 0.0160 0.0127 C3 0.0309 0.0176 0.0127 C4 0.0282 0.0179 0.0128 C5 0.0212 0.0155 0.0150 C6 0.0238 0.0183 0.0149 C7 0.0266 0.0169 0.0144 C8 0.0327 0.0232 0.0140 C9 0.0589 0.0320 0.0147 C10 0.0178 0.0162 0.0136 C11 0.0257 0.0194 0.0142 C12 0.0371 0.0214 0.0159 C13 0.0534 0.0271 0.0156 C14 0.0264 0.0190 0.0146 C15 0.0168 0.0155 0.0115 N1 0.0522 0.0311 0.0172 N2 0.0680 0.0215 0.0135 O1 0.0324 0.0188 0.0154 O2 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.011 0.023 0.035 0.049 0.063 0.082 0.104 0.133 0.196 1.000 Number in group 341. 318. 334. 305. 328. 327. 322. 310. 325. 324. GooF 1.094 1.033 0.981 1.104 1.087 0.955 1.060 1.001 1.017 0.992 K 3.034 1.232 1.048 1.037 0.995 1.006 0.997 0.998 1.005 0.993 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.04 1.15 1.31 1.63 inf Number in group 339. 312. 326. 322. 320. 322. 329. 320. 318. 326. GooF 0.911 0.970 0.989 0.892 0.958 0.960 1.053 0.938 1.190 1.375 K 1.031 1.029 1.016 0.994 0.998 0.994 1.005 1.005 1.017 0.983 R1 0.085 0.088 0.080 0.059 0.054 0.046 0.037 0.031 0.037 0.033 Recommended weighting scheme: WGHT 0.0418 0.5176 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) 0 2 1 413.40 639.21 4.47 0.237 6.61 -2 7 8 13.50 32.53 4.37 0.054 1.13 1 2 0 6260.62 7752.25 3.85 0.826 5.88 0 5 5 53.09 34.12 3.70 0.055 1.73 0 12 0 33.73 14.49 3.64 0.036 1.48 -1 3 6 12.36 4.58 3.60 0.020 1.63 -7 1 5 100.23 141.03 3.59 0.111 1.08 0 7 5 250.21 198.08 3.54 0.132 1.56 -2 5 5 411.37 333.76 3.54 0.171 1.71 2 7 3 69.87 48.06 3.53 0.065 1.70 3 0 3 5.26 15.41 3.49 0.037 1.87 -10 1 3 93.55 58.72 3.45 0.072 0.80 -6 0 2 24.17 11.13 3.42 0.031 1.34 -3 0 3 123.34 93.19 3.33 0.091 2.31 -6 17 1 84.67 125.75 3.27 0.105 0.82 0 7 8 56.89 37.83 3.24 0.058 1.11 -2 6 5 9.86 1.23 3.23 0.010 1.62 0 0 2 3957.81 4625.90 3.17 0.638 4.96 -2 4 2 33.60 21.16 3.14 0.043 2.73 -8 7 1 17.36 31.70 3.13 0.053 0.93 -1 5 4 30.86 18.68 3.10 0.041 2.06 9 3 3 52.48 31.68 3.09 0.053 0.80 -8 6 4 27.18 15.00 3.05 0.036 0.94 1 0 1 1417.60 1737.30 3.03 0.391 5.61 0 15 8 78.00 116.69 3.03 0.101 0.86 -1 3 1 2902.39 3419.38 2.98 0.549 4.49 3 0 5 6.45 1.15 2.97 0.010 1.44 -3 6 4 101.81 77.66 2.95 0.083 1.67 -1 13 2 3.42 0.13 2.95 0.003 1.31 -8 6 3 75.76 101.15 2.92 0.094 0.95 -4 7 5 274.83 226.95 2.89 0.141 1.34 -1 8 8 20.01 32.14 2.79 0.053 1.10 -2 9 11 137.10 106.21 2.79 0.097 0.84 -2 15 7 11.70 4.31 2.79 0.019 0.91 1 7 4 484.52 414.97 2.79 0.191 1.67 -7 3 6 39.31 56.35 2.78 0.070 1.02 4 3 0 205.04 168.31 2.77 0.122 1.87 -4 10 8 20.99 33.49 2.76 0.054 0.97 8 1 1 35.62 21.09 2.76 0.043 0.96 1 3 1 1516.22 1725.58 2.70 0.390 4.07 -8 5 8 31.36 18.26 2.70 0.040 0.84 1 3 9 14.18 6.43 2.69 0.024 1.04 1 1 1 606.17 698.23 2.63 0.248 5.35 -7 5 4 4.26 10.98 2.63 0.031 1.07 -2 11 7 224.53 268.61 2.63 0.154 1.07 -3 3 2 66.10 49.77 2.63 0.066 2.34 3 3 6 3.45 0.00 2.63 0.000 1.25 2 5 2 48.54 35.24 2.62 0.056 2.20 0 3 9 9.28 4.06 2.61 0.019 1.08 0 17 8 15.38 5.68 2.60 0.022 0.80 Bond lengths and angles C1 - Distance Angles C6 1.3836 (0.0015) C2 1.3996 (0.0015) 120.13 (0.10) N1 1.4450 (0.0013) 120.39 (0.09) 119.48 (0.09) C1 - C6 C2 C2 - Distance Angles C3 1.3968 (0.0015) C1 1.3996 (0.0015) 120.24 (0.10) C15 1.4383 (0.0015) 121.34 (0.10) 118.43 (0.09) C2 - C3 C1 C3 - Distance Angles C4 1.3866 (0.0016) C2 1.3968 (0.0015) 119.41 (0.10) H3 0.9500 120.29 120.30 C3 - C4 C2 C4 - Distance Angles C3 1.3866 (0.0016) C5 1.3911 (0.0017) 120.23 (0.10) H4 0.9500 119.89 119.89 C4 - C3 C5 C5 - Distance Angles C4 1.3911 (0.0017) C6 1.3956 (0.0015) 120.51 (0.10) H5 0.9500 119.75 119.75 C5 - C4 C6 C6 - Distance Angles C1 1.3836 (0.0015) C5 1.3956 (0.0015) 119.47 (0.10) H6 0.9500 120.26 120.26 C6 - C1 C5 C7 - Distance Angles O1 1.2100 (0.0014) N1 1.4117 (0.0014) 122.22 (0.10) C8 1.5129 (0.0015) 121.76 (0.10) 116.02 (0.09) C7 - O1 N1 C8 - Distance Angles C7 1.5129 (0.0015) C9 1.5224 (0.0015) 111.55 (0.09) H8A 0.9900 109.31 109.31 H8B 0.9900 109.31 109.31 107.96 C8 - C7 C9 H8A C9 - Distance Angles C8 1.5224 (0.0015) C10 1.5232 (0.0017) 112.33 (0.10) H9A 0.9900 109.14 109.14 H9B 0.9900 109.14 109.14 107.86 C9 - C8 C10 H9A C10 - Distance Angles C9 1.5232 (0.0017) H10A 0.9800 109.47 H10B 0.9800 109.47 109.47 H10C 0.9800 109.47 109.47 109.47 C10 - C9 H10A H10B C11 - Distance Angles O2 1.2132 (0.0014) N1 1.4191 (0.0013) 118.03 (0.09) C12 1.5066 (0.0014) 122.50 (0.10) 119.46 (0.09) C11 - O2 N1 C12 - Distance Angles C11 1.5066 (0.0014) C13 1.5216 (0.0015) 112.62 (0.09) H12A 0.9900 109.07 109.07 H12B 0.9900 109.07 109.07 107.82 C12 - C11 C13 H12A C13 - Distance Angles C12 1.5216 (0.0015) C14 1.5246 (0.0016) 110.25 (0.10) H13A 0.9900 109.61 109.61 H13B 0.9900 109.61 109.61 108.13 C13 - C12 C14 H13A C14 - Distance Angles C13 1.5246 (0.0016) H14A 0.9800 109.47 H14B 0.9800 109.47 109.47 H14C 0.9800 109.47 109.47 109.47 C14 - C13 H14A H14B C15 - Distance Angles N2 1.1468 (0.0016) C2 1.4383 (0.0015) 177.77 (0.13) C15 - N2 N1 - Distance Angles C7 1.4117 (0.0014) C11 1.4191 (0.0013) 125.48 (0.09) C1 1.4450 (0.0013) 119.30 (0.08) 115.21 (0.08) N1 - C7 C11 N2 - Distance Angles C15 1.1468 (0.0016) N2 - O1 - Distance Angles C7 1.2100 (0.0014) O1 - O2 - Distance Angles C11 1.2132 (0.0014) O2 - FMAP and GRID set by program FMAP 2 2 23 GRID -1.250 -2 -2 1.250 2 2 R1 = 0.0479 for 3234 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.28 at 0.1982 0.0282 0.4527 [ 0.85 A from O1 ] Deepest hole -0.22 at 0.4004 0.0474 0.4907 [ 0.77 A from O1 ] Mean = 0.00, Rms deviation from mean = 0.04 e/A^3, Highest memory used = 2230 / 18336 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.8018 -0.0282 0.5473 1.00000 0.05 0.28 0.85 O1 1.33 C7 2.19 H12B 2.27 N1 Q2 1 0.7215 -0.0023 0.6955 1.00000 0.05 0.26 0.72 C8 0.79 C7 1.40 H8B 1.42 H8A Q3 1 0.7282 -0.0542 0.7742 1.00000 0.05 0.23 0.74 C8 0.79 C9 1.38 H8A 1.41 H9B Q4 1 0.7641 0.1543 0.7421 1.00000 0.05 0.23 0.69 C2 0.72 C1 1.84 C3 1.85 C6 Q5 1 0.7565 -0.1096 0.8555 1.00000 0.05 0.23 0.74 C9 0.78 C10 1.42 H9A 1.42 H9B Shortest distances between peaks (including symmetry equivalents) 2 3 1.21 3 5 1.27 1 2 1.82 2 5 2.48 1 3 2.54 2 4 2.82 Time profile in seconds ----------------------- 0.06: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.00: Generate connectivity array 0.00: Analyse DFIX/DANG restraints 0.00: Analyse SAME/SADI restraints 0.00: Generate CHIV restraints 0.00: Check if bonds in residues restrained 0.00: Generate DELU restraints 0.00: Generate SIMU restraints 0.00: Generate ISOR restraints 0.00: Generate NCSY restraints 0.00: Analyse other restraints etc. 1.02: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.02: Set up l.s. refinement 0.00: Generate idealized H-atoms 1.00: Structure factors and derivatives 1.03: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.03: Apply other restraints 0.17: Solve l.s. equations 0.00: Generate HTAB table 0.00: Other dependent quantities, CIF, tables 0.05: Analysis of variance 0.03: Merge reflections for Fourier and .fcf 0.05: Fourier summations 0.00: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + shelxl finished at 13:32:52 Total CPU time: 3.5 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++