+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXH-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + s92 started at 15:50:56 on 08-Mar-2004 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL s92 in P2(1)/c CELL 0.71073 3.7872 14.5657 22.4435 90.000 91.700 90.000 ZERR 4.00 0.0003 0.0011 0.0021 0.000 0.003 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N CL CU SE UNIT 36 24 4 12 12 4 V = 1237.51 F(000) = 956.0 Mu = 8.67 mm-1 Cell Wt = 2016.31 Rho = 2.706 MERG 2 OMIT -3.00 55.00 SHEL 7 0.77 FMAP 2 PLAN 5 SIZE 0.02 0.05 0.22 ACTA BOND $H WGHT 0.01890 27.27060 L.S. 12 TEMP -153.00 FVAR 0.13173 C1 1 0.203389 0.081227 0.286302 11.00000 0.02137 0.03512 = 0.02643 -0.01015 -0.00516 -0.00725 C2 1 0.334900 0.074420 0.230394 11.00000 0.02023 0.04738 = 0.02389 -0.00241 -0.00511 0.00619 AFIX 43 H2 2 0.363542 0.127849 0.206747 11.00000 -1.20000 AFIX 0 C3 1 0.426479 -0.011424 0.208405 11.00000 0.02469 0.05740 = 0.02058 -0.00413 -0.00045 -0.00766 AFIX 43 H3 2 0.514461 -0.015281 0.169283 11.00000 -1.20000 AFIX 0 C4 1 0.395772 -0.088974 0.240121 11.00000 0.01934 0.04073 = 0.02948 -0.01248 0.00135 0.00258 AFIX 43 H4 2 0.477286 -0.145584 0.224626 11.00000 -1.20000 AFIX 0 C5 1 0.239782 -0.086022 0.297353 11.00000 0.02848 0.04012 = 0.03413 -0.00666 -0.00648 0.00131 C6 1 0.146943 0.001504 0.321676 11.00000 0.01915 0.05414 = 0.02136 -0.00361 -0.00891 -0.00231 C7 1 -0.030843 -0.068238 0.408521 11.00000 0.01766 0.02873 = 0.02506 0.00500 -0.00241 -0.00247 AFIX 43 H7 2 -0.118969 -0.062844 0.447557 11.00000 -1.20000 AFIX 0 C8 1 0.042502 -0.155962 0.387006 11.00000 0.04473 0.02894 = 0.03352 0.01267 -0.01523 -0.00284 AFIX 43 H8 2 -0.006078 -0.208924 0.410067 11.00000 -1.20000 AFIX 0 C9 1 0.185931 -0.163975 0.331960 11.00000 0.01803 0.03572 = 0.05332 0.00047 -0.01539 0.00110 AFIX 43 H9 2 0.248859 -0.222760 0.317324 11.00000 -1.20000 AFIX 0 N1 3 0.015704 0.007452 0.377547 11.00000 0.02883 0.02709 = 0.02361 -0.00166 -0.00068 -0.00155 CL1 4 -0.505765 0.168707 0.471211 11.00000 0.02540 0.03685 = 0.02684 0.00157 0.00223 -0.00132 CL2 4 -0.485749 0.374712 0.573314 11.00000 0.03452 0.03356 = 0.04295 -0.01148 0.00322 0.00045 CL3 4 -1.000687 0.612537 0.576233 11.00000 0.03212 0.03557 = 0.05483 0.01408 0.00072 0.00000 CU1 5 -0.038461 0.124778 0.420618 11.00000 0.04435 0.03819 = 0.03109 -0.00176 0.00684 0.00314 CU2 5 -0.489027 0.327225 0.472018 11.00000 0.04999 0.05516 = 0.04701 0.00856 0.00305 0.00155 CU3 5 -0.984002 0.460954 0.561307 11.00000 0.04138 0.04881 = 0.04799 0.00772 0.00456 0.00279 SE1 6 0.069206 0.197484 0.316293 11.00000 0.03103 0.02827 = 0.02708 0.00260 0.00457 0.00056 HKLF 4 Covalent radii and connectivity table for s92 in P2(1)/c C 0.770 H 0.320 N 0.700 CL 0.990 CU 1.280 SE 1.170 C1 - C2 C6 Se1 C2 - C1 C3 C3 - C4 C2 C4 - C3 C5 C5 - C9 C4 C6 C6 - N1 C1 C5 C7 - N1 C8 C8 - C9 C7 C9 - C8 C5 N1 - C7 C6 Cu1 Cl1 - Cu1 Cu2 Cu1_$2 Cl2 - Cu3 Cu3_$1 Cu2 Cl3 - Cu3 Cu2_$4 Cu2_$3 Cu1 - N1 Cl1 Cl1_$1 Se1 Cu2 - Cl1 Cl3_$4 Cl3_$3 Cl2 Cu3 - Cl3 Cl2 Cl2_$2 Cu3_$3 Se1 - C1 Cu1 Operators for generating equivalent atoms: $1 x+1, y, z $2 x-1, y, z $3 -x-2, -y+1, -z+1 $4 -x-1, -y+1, -z+1 h k l Fo^2 Sigma Why rejected 3 0 5 15.89 2.27 observed but should be systematically absent -3 0 5 23.86 4.55 observed but should be systematically absent 2 0 7 14.89 3.44 observed but should be systematically absent 2 0 5 24.02 3.43 observed but should be systematically absent 2 0 1 36.63 6.87 observed but should be systematically absent -2 0 5 24.99 5.68 observed but should be systematically absent 1 0 5 4.58 1.14 observed but should be systematically absent 1 0 5 5.71 1.14 observed but should be systematically absent -1 0 1 5.66 1.13 observed but should be systematically absent 1 0 5 5.72 1.14 observed but should be systematically absent 2 0 1 41.20 6.87 observed but should be systematically absent 2 0 3 10.31 2.29 observed but should be systematically absent 2 0 3 20.40 4.53 observed but should be systematically absent 2 0 3 9.12 1.14 observed but should be systematically absent -3 0 7 14.26 3.29 observed but should be systematically absent -3 0 5 34.21 4.57 observed but should be systematically absent -3 0 5 28.38 3.29 observed but should be systematically absent 3 0 5 18.16 3.41 observed but should be systematically absent 3 0 7 19.47 4.58 observed but should be systematically absent 11653 Reflections read, of which 301 rejected -4 =< h =< 4, -18 =< k =< 18, -29 =< l =< 29, Max. 2-theta = 54.84 19 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 0 2 1 91.14 1.08 7 24.46 2 11 1 13.84 1.88 3 11.61 0 1 3 292.65 6.36 4 137.64 2 7 3 18.11 0.94 5 5.53 2 8 3 17.81 1.08 6 16.46 3 4 8 6.37 1.18 6 8.54 0 15 17 20.09 7.64 2 38.96 0 11 23 8.07 3.55 3 23.93 0 9 25 3.14 2.87 4 15.23 0 6 27 29.07 7.96 2 48.72 10 Inconsistent equivalents 2739 Unique reflections, of which 0 suppressed R(int) = 0.0929 R(sigma) = 0.1083 Friedel opposites merged Maximum memory for data reduction = 1646 / 26885 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 = 2040 / 194670 wR2 = 0.1764 before cycle 1 for 2739 data and 154 / 154 parameters GooF = S = 1.153; Restrained GooF = 1.153 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0189 * P )^2 + 27.27 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.13170 0.00043 -0.066 OSF Mean shift/esd = 0.008 Maximum = -0.066 for OSF Max. shift = 0.000 A for C8 Max. dU = 0.000 for C3 Least-squares cycle 2 Maximum vector length = 511 Memory required = 2040 / 194670 wR2 = 0.1764 before cycle 2 for 2739 data and 154 / 154 parameters GooF = S = 1.154; Restrained GooF = 1.154 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0189 * P )^2 + 27.27 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.13169 0.00043 -0.023 OSF Mean shift/esd = 0.003 Maximum = -0.023 for OSF Max. shift = 0.000 A for C5 Max. dU = 0.000 for C3 Least-squares cycle 3 Maximum vector length = 511 Memory required = 2040 / 194670 wR2 = 0.1764 before cycle 3 for 2739 data and 154 / 154 parameters GooF = S = 1.154; Restrained GooF = 1.154 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0189 * P )^2 + 27.27 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.13169 0.00043 -0.001 OSF Mean shift/esd = 0.000 Maximum = -0.002 for U11 Cl3 Max. shift = 0.000 A for C5 Max. dU = 0.000 for C9 Least-squares cycle 4 Maximum vector length = 511 Memory required = 2040 / 194670 wR2 = 0.1764 before cycle 4 for 2739 data and 154 / 154 parameters GooF = S = 1.154; Restrained GooF = 1.154 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0189 * P )^2 + 27.27 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.13169 0.00043 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.001 for U11 Cl3 Max. shift = 0.000 A for C9 Max. dU = 0.000 for C9 Least-squares cycle 5 Maximum vector length = 511 Memory required = 2040 / 194670 wR2 = 0.1764 before cycle 5 for 2739 data and 154 / 154 parameters GooF = S = 1.154; Restrained GooF = 1.154 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0189 * P )^2 + 27.27 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.13169 0.00043 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for C9 Max. dU = 0.000 for C3 Least-squares cycle 6 Maximum vector length = 511 Memory required = 2040 / 194670 wR2 = 0.1764 before cycle 6 for 2739 data and 154 / 154 parameters GooF = S = 1.154; Restrained GooF = 1.154 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0189 * P )^2 + 27.27 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.13169 0.00043 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for z Cu3 Max. shift = 0.000 A for C6 Max. dU = 0.000 for C9 Least-squares cycle 7 Maximum vector length = 511 Memory required = 2040 / 194670 wR2 = 0.1764 before cycle 7 for 2739 data and 154 / 154 parameters GooF = S = 1.154; Restrained GooF = 1.154 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0189 * P )^2 + 27.27 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.13169 0.00043 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for z Cu3 Max. shift = 0.000 A for C2 Max. dU = 0.000 for C3 Least-squares cycle 8 Maximum vector length = 511 Memory required = 2040 / 194670 wR2 = 0.1764 before cycle 8 for 2739 data and 154 / 154 parameters GooF = S = 1.154; Restrained GooF = 1.154 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0189 * P )^2 + 27.27 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.13169 0.00043 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for z Cu3 Max. shift = 0.000 A for C7 Max. dU = 0.000 for C7 Least-squares cycle 9 Maximum vector length = 511 Memory required = 2040 / 194670 wR2 = 0.1764 before cycle 9 for 2739 data and 154 / 154 parameters GooF = S = 1.154; Restrained GooF = 1.154 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0189 * P )^2 + 27.27 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.13169 0.00043 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for z Cu3 Max. shift = 0.000 A for C8 Max. dU = 0.000 for C3 Least-squares cycle 10 Maximum vector length = 511 Memory required = 2040 / 194670 wR2 = 0.1764 before cycle 10 for 2739 data and 154 / 154 parameters GooF = S = 1.154; Restrained GooF = 1.154 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0189 * P )^2 + 27.27 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.13169 0.00043 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for z Cl2 Max. shift = 0.000 A for C6 Max. dU = 0.000 for C8 Least-squares cycle 11 Maximum vector length = 511 Memory required = 2040 / 194670 wR2 = 0.1764 before cycle 11 for 2739 data and 154 / 154 parameters GooF = S = 1.154; Restrained GooF = 1.154 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0189 * P )^2 + 27.27 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.13169 0.00043 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for z Cu3 Max. shift = 0.000 A for H7 Max. dU = 0.000 for N1 Least-squares cycle 12 Maximum vector length = 511 Memory required = 2040 / 194670 wR2 = 0.1764 before cycle 12 for 2739 data and 154 / 154 parameters GooF = S = 1.154; Restrained GooF = 1.154 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0189 * P )^2 + 27.27 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.13169 0.00043 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for z Cu3 Max. shift = 0.000 A for C4 Max. dU = 0.000 for N1 No correlation matrix elements larger than 0.500 Idealized hydrogen atom generation before cycle 13 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2 0.3637 0.1278 0.2068 43 0.950 0.000 C2 C1 C3 H3 0.5143 -0.0153 0.1693 43 0.950 0.000 C3 C4 C2 H4 0.4773 -0.1456 0.2246 43 0.950 0.000 C4 C3 C5 H7 -0.1189 -0.0629 0.4476 43 0.950 0.000 C7 N1 C8 H8 -0.0059 -0.2089 0.4101 43 0.950 0.000 C8 C9 C7 H9 0.2488 -0.2228 0.3173 43 0.950 0.000 C9 C8 C5 s92 in P2(1)/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.20336 0.08124 0.28629 1.00000 0.02142 0.03506 0.02640 -0.01021 -0.00509 -0.00729 0.02775 0.01934 0.00314 0.00088 0.00053 0.00000 0.00663 0.00728 0.00635 0.00558 0.00510 0.00589 0.00285 C2 0.33492 0.07441 0.23040 1.00000 0.02032 0.04719 0.02388 -0.00229 -0.00503 0.00621 0.03058 0.02163 0.00316 0.00098 0.00053 0.00000 0.00651 0.00826 0.00627 0.00594 0.00508 0.00626 0.00298 H2 0.36367 0.12784 0.20676 1.00000 0.03669 0.00000 0.00000 C3 0.42641 -0.01143 0.20841 1.00000 0.02475 0.05756 0.02052 -0.00403 -0.00046 -0.00773 0.03430 0.02147 0.00328 0.00100 0.00055 0.00000 0.00721 0.00937 0.00612 0.00632 0.00535 0.00678 0.00326 H3 0.51429 -0.01528 0.16928 1.00000 0.04116 0.00000 0.00000 C4 0.39578 -0.08898 0.24011 1.00000 0.01922 0.04068 0.02952 -0.01251 0.00131 0.00266 0.02979 0.02087 0.00311 0.00094 0.00054 0.00000 0.00656 0.00788 0.00666 0.00603 0.00526 0.00609 0.00297 H4 0.47734 -0.14558 0.22462 1.00000 0.03575 0.00000 0.00000 C5 0.23978 -0.08604 0.29736 1.00000 0.02848 0.04010 0.03402 -0.00673 -0.00645 0.00133 0.03435 0.02201 0.00342 0.00095 0.00058 0.00000 0.00752 0.00806 0.00721 0.00631 0.00586 0.00653 0.00317 C6 0.14695 0.00149 0.32168 1.00000 0.01917 0.05408 0.02141 -0.00363 -0.00897 -0.00225 0.03175 0.02076 0.00319 0.00098 0.00052 0.00000 0.00657 0.00881 0.00625 0.00609 0.00518 0.00634 0.00310 C7 -0.03079 -0.06824 0.40851 1.00000 0.01763 0.02867 0.02518 0.00492 -0.00242 -0.00244 0.02389 0.02014 0.00299 0.00082 0.00053 0.00000 0.00620 0.00667 0.00609 0.00523 0.00492 0.00547 0.00263 H7 -0.11892 -0.06285 0.44755 1.00000 0.02866 0.00000 0.00000 C8 0.04259 -0.15597 0.38700 1.00000 0.04470 0.02891 0.03352 0.01268 -0.01525 -0.00284 0.03603 0.02258 0.00367 0.00091 0.00059 0.00000 0.00853 0.00713 0.00754 0.00597 0.00652 0.00663 0.00335 H8 -0.00592 -0.20893 0.41007 1.00000 0.04324 0.00000 0.00000 C9 0.18593 -0.16399 0.33197 1.00000 0.01794 0.03570 0.05334 0.00049 -0.01534 0.00109 0.03598 0.02258 0.00320 0.00097 0.00065 0.00000 0.00655 0.00757 0.00899 0.00670 0.00623 0.00613 0.00331 H9 0.24882 -0.22277 0.31733 1.00000 0.04318 0.00000 0.00000 N1 0.01570 0.00746 0.37754 1.00000 0.02894 0.02701 0.02363 -0.00159 -0.00072 -0.00152 0.02655 0.01669 0.00264 0.00068 0.00042 0.00000 0.00593 0.00557 0.00520 0.00441 0.00446 0.00480 0.00233 Cl1 -0.50577 0.16870 0.47121 1.00000 0.02539 0.03683 0.02683 0.00156 0.00222 -0.00135 0.02965 0.00534 0.00079 0.00022 0.00013 0.00000 0.00156 0.00175 0.00154 0.00128 0.00124 0.00142 0.00070 Cl2 -0.48574 0.37471 0.57331 1.00000 0.03445 0.03355 0.04293 -0.01149 0.00320 0.00044 0.03694 0.00562 0.00089 0.00023 0.00015 0.00000 0.00185 0.00179 0.00190 0.00148 0.00149 0.00154 0.00080 Cl3 -1.00070 0.61254 0.57623 1.00000 0.03205 0.03556 0.05483 0.01409 0.00073 0.00000 0.04082 0.00634 0.00090 0.00024 0.00016 0.00000 0.00189 0.00188 0.00217 0.00164 0.00161 0.00159 0.00086 Cu1 -0.03846 0.12478 0.42062 1.00000 0.04432 0.03814 0.03106 -0.00176 0.00684 0.00315 0.03772 0.00303 0.00047 0.00012 0.00007 0.00000 0.00106 0.00098 0.00089 0.00074 0.00075 0.00084 0.00046 Cu2 -0.48902 0.32722 0.47202 1.00000 0.04997 0.05513 0.04697 0.00854 0.00304 0.00156 0.05066 0.00356 0.00052 0.00014 0.00009 0.00000 0.00118 0.00125 0.00114 0.00091 0.00090 0.00099 0.00055 Cu3 -0.98399 0.46095 0.56131 1.00000 0.04134 0.04878 0.04796 0.00772 0.00456 0.00280 0.04596 0.00339 0.00049 0.00013 0.00008 0.00000 0.00110 0.00116 0.00111 0.00088 0.00086 0.00091 0.00053 Se1 0.06921 0.19748 0.31629 1.00000 0.03100 0.02826 0.02706 0.00260 0.00457 0.00056 0.02870 0.00230 0.00035 0.00009 0.00006 0.00000 0.00070 0.00065 0.00063 0.00056 0.00051 0.00060 0.00033 Final Structure Factor Calculation for s92 in P2(1)/c Total number of l.s. parameters = 154 Maximum vector length = 511 Memory required = 1886 / 25039 wR2 = 0.1764 before cycle 13 for 2739 data and 0 / 154 parameters GooF = S = 1.154; Restrained GooF = 1.154 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0189 * P )^2 + 27.27 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0877 for 1838 Fo > 4sig(Fo) and 0.1417 for all 2739 data wR2 = 0.1764, GooF = S = 1.154, Restrained GooF = 1.154 for all data Occupancy sum of asymmetric unit = 17.00 for non-hydrogen and 6.00 for hydrogen atoms Principal mean square atomic displacements U 0.0422 0.0292 0.0118 C1 0.0491 0.0268 0.0158 C2 0.0596 0.0241 0.0192 C3 0.0490 0.0225 0.0179 C4 0.0463 0.0337 0.0231 C5 0.0545 0.0302 0.0106 C6 0.0332 0.0219 0.0166 C7 0.0603 0.0323 0.0155 C8 0.0603 0.0358 0.0119 C9 0.0299 0.0274 0.0225 N1 0.0372 0.0276 0.0241 Cl1 0.0507 0.0346 0.0255 Cl2 0.0623 0.0320 0.0281 Cl3 0.0469 0.0383 0.0280 Cu1 0.0609 0.0496 0.0415 Cu2 0.0571 0.0409 0.0398 Cu3 0.0338 0.0286 0.0238 Se1 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.013 0.024 0.036 0.050 0.062 0.078 0.099 0.131 0.195 1.000 Number in group 290. 279. 267. 282. 255. 280. 275. 265. 271. 275. GooF 1.288 1.639 1.265 1.071 1.039 0.941 0.971 0.989 0.956 1.167 K 19.743 4.573 2.200 1.434 1.293 1.126 1.057 1.031 0.988 0.987 Resolution(A) 0.77 0.80 0.84 0.88 0.92 0.98 1.06 1.16 1.32 1.68 inf Number in group 281. 277. 270. 277. 265. 276. 272. 273. 276. 272. GooF 0.946 1.024 1.027 0.972 1.007 1.068 1.301 1.307 1.084 1.629 K 1.553 1.426 1.235 1.110 1.128 1.013 1.017 0.972 0.998 1.002 R1 0.380 0.329 0.271 0.192 0.175 0.137 0.104 0.084 0.057 0.051 Recommended weighting scheme: WGHT 0.0194 27.2773 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 1 1120.52 113.73 7.11 0.030 1.24 3 7 3 1315.92 48.87 7.05 0.020 1.06 3 3 6 961.84 49.86 6.54 0.020 1.15 -3 1 7 895.65 24.05 5.95 0.014 1.18 0 5 1 648.86 68.58 5.86 0.023 2.89 2 4 1 1527.46 525.80 4.59 0.064 1.67 -3 1 11 1317.63 341.28 4.41 0.052 1.08 -1 6 3 515.48 81.62 4.07 0.025 1.98 3 7 1 618.92 32.80 4.05 0.016 1.08 3 6 1 364.78 8.42 4.01 0.008 1.12 1 0 2 307.07 24.89 4.00 0.014 3.55 1 1 0 362.92 51.87 3.92 0.020 3.66 0 0 4 2375.86 1263.13 3.90 0.099 5.61 3 8 2 502.61 35.83 3.86 0.017 1.03 2 1 5 3939.35 2530.13 3.84 0.141 1.71 -2 8 7 490.17 6.86 3.84 0.007 1.22 0 3 5 2089.96 1149.33 3.80 0.095 3.30 -1 1 3 2409.81 1335.62 3.77 0.102 3.33 -1 2 3 367.25 60.38 3.73 0.022 3.09 0 2 7 2039.81 1196.10 3.57 0.097 2.93 0 4 4 205.32 6.40 3.46 0.007 3.05 -1 1 4 6629.07 4960.74 3.35 0.197 3.11 -3 1 3 572.63 165.75 3.33 0.036 1.25 1 0 4 102153.55 117508.07 3.21 0.958 3.10 3 5 3 288.99 1.98 3.14 0.004 1.14 1 2 3 319.98 75.07 3.11 0.024 3.03 4 3 6 807.54 36.64 3.08 0.017 0.90 -3 2 1 547.15 187.27 3.08 0.038 1.24 -3 5 11 711.59 196.06 3.08 0.039 1.02 0 4 1 4135.38 3017.98 3.06 0.153 3.59 3 3 2 248.15 18.07 3.05 0.012 1.21 -3 6 4 767.00 235.01 3.04 0.043 1.10 -2 3 2 257.50 5.60 2.90 0.007 1.75 -4 2 3 705.46 134.14 2.87 0.032 0.93 0 6 6 18388.67 15601.19 2.83 0.349 2.04 -2 7 9 1064.34 440.39 2.83 0.059 1.23 -1 2 8 349.95 67.91 2.83 0.023 2.18 4 1 5 511.19 27.84 2.82 0.015 0.92 3 1 8 710.03 284.01 2.81 0.047 1.13 2 5 5 444.71 142.83 2.77 0.033 1.48 -3 2 6 500.45 146.17 2.71 0.034 1.19 1 4 9 436.80 171.36 2.67 0.037 1.79 3 2 9 740.70 340.01 2.63 0.052 1.10 2 3 6 672.69 305.79 2.63 0.049 1.58 -4 3 10 1159.30 424.89 2.62 0.058 0.87 3 5 0 1499.44 807.98 2.61 0.079 1.16 0 2 12 312.34 62.45 2.60 0.022 1.81 3 9 4 1052.32 53.00 2.59 0.020 0.98 0 3 2 3348.17 2502.89 2.56 0.140 4.46 -1 12 6 321.61 33.82 2.56 0.016 1.11 Bond lengths and angles C1 - Distance Angles C2 1.3670 (0.0164) C6 1.4268 (0.0181) 121.07 (1.20) Se1 1.8969 (0.0125) 119.96 (1.03) 118.89 (0.90) C1 - C2 C6 C2 - Distance Angles C1 1.3670 (0.0164) C3 1.3919 (0.0187) 119.48 (1.30) H2 0.9500 120.26 120.26 C2 - C1 C3 C3 - Distance Angles C4 1.3419 (0.0183) C2 1.3919 (0.0187) 122.80 (1.22) H3 0.9500 118.60 118.60 C3 - C4 C2 C4 - Distance Angles C3 1.3419 (0.0183) C5 1.4306 (0.0175) 119.71 (1.23) H4 0.9500 120.15 120.15 C4 - C3 C5 C5 - Distance Angles C9 1.3940 (0.0191) C4 1.4306 (0.0175) 123.17 (1.29) C6 1.4347 (0.0185) 118.05 (1.25) 118.72 (1.25) C5 - C9 C4 C6 - Distance Angles N1 1.3652 (0.0150) C1 1.4268 (0.0181) 121.60 (1.19) C5 1.4347 (0.0185) 120.39 (1.22) 118.00 (1.12) C6 - N1 C1 C7 - Distance Angles N1 1.3180 (0.0146) C8 1.3968 (0.0178) 123.50 (1.14) H7 0.9500 118.25 118.25 C7 - N1 C8 C8 - Distance Angles C9 1.3689 (0.0194) C7 1.3968 (0.0178) 118.57 (1.22) H8 0.9500 120.72 120.72 C8 - C9 C7 C9 - Distance Angles C8 1.3689 (0.0194) C5 1.3940 (0.0191) 120.12 (1.32) H9 0.9500 119.94 119.94 C9 - C8 C5 N1 - Distance Angles C7 1.3180 (0.0146) C6 1.3652 (0.0150) 119.28 (1.10) Cu1 1.9770 (0.0099) 116.60 (0.80) 123.37 (0.87) N1 - C7 C6 Cl1 - Distance Angles Cu1 2.2249 (0.0035) Cu2 2.3099 (0.0038) 105.63 (0.14) Cu1_$2 2.3734 (0.0035) 110.86 (0.14) 107.22 (0.14) Cl1 - Cu1 Cu2 Cl2 - Distance Angles Cu3 2.2762 (0.0039) Cu3_$1 2.3004 (0.0039) 111.69 (0.16) Cu2 2.3760 (0.0039) 93.82 (0.14) 91.59 (0.14) Cl2 - Cu3 Cu3_$1 Cl3 - Distance Angles Cu3 2.2344 (0.0040) Cu2_$4 2.3455 (0.0040) 105.91 (0.16) Cu2_$3 2.3565 (0.0039) 109.00 (0.16) 107.31 (0.15) Cl3 - Cu3 Cu2_$4 Cu1 - Distance Angles N1 1.9770 (0.0099) Cl1 2.2249 (0.0035) 126.43 (0.32) Cl1_$1 2.3734 (0.0035) 111.59 (0.31) 110.86 (0.14) Se1 2.6128 (0.0021) 83.74 (0.29) 119.24 (0.11) 99.58 (0.10) Cu1 - N1 Cl1 Cl1_$1 Cu2 - Distance Angles Cl1 2.3099 (0.0038) Cl3_$4 2.3455 (0.0040) 113.09 (0.14) Cl3_$3 2.3565 (0.0039) 110.28 (0.14) 107.31 (0.15) Cl2 2.3760 (0.0039) 107.33 (0.14) 110.55 (0.15) 108.19 (0.15) Cu2 - Cl1 Cl3_$4 Cl3_$3 Cu3 - Distance Angles Cl3 2.2344 (0.0040) Cl2 2.2762 (0.0039) 123.69 (0.15) Cl2_$2 2.3004 (0.0040) 119.66 (0.15) 111.69 (0.16) Cu3_$3 2.9769 (0.0037) 76.14 (0.12) 109.34 (0.13) 107.81 (0.13) Cu3 - Cl3 Cl2 Cl2_$2 Se1 - Distance Angles C1 1.8969 (0.0125) Cu1 2.6128 (0.0021) 90.39 (0.39) Se1 - C1 FMAP and GRID set by program FMAP 2 1 12 GRID -5.556 -2 -1 5.556 2 1 R1 = 0.1362 for 2739 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 1.94 at 0.1939 0.6954 0.1853 [ 1.00 A from SE1 ] Deepest hole -0.88 at 0.0542 0.0980 0.4082 [ 0.60 A from CU1 ] Mean = 0.00, Rms deviation from mean = 0.21 e/A^3, Highest memory used = 2772 / 28824 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 -0.1939 0.1954 0.3147 1.00000 0.05 1.94 1.00 SE1 2.34 C1 2.64 CU1 2.69 H4 Q2 1 0.2632 0.1262 0.4205 1.00000 0.05 1.42 1.14 CU1 1.54 CL1 2.18 N1 2.64 SE1 Q3 1 -1.0149 0.4397 0.5236 1.00000 0.05 0.93 0.91 CU3 2.33 CL2 2.37 CL3 2.39 CU3 Q4 1 -1.2525 0.4635 0.5613 1.00000 0.05 0.88 1.02 CU3 1.59 CL2 2.39 CL3 2.71 H3 Q5 1 0.0639 0.2421 0.3128 1.00000 0.05 0.85 0.65 SE1 2.48 C1 2.55 H4 3.00 CU1 Shortest distances between peaks (including symmetry equivalents) 1 5 1.19 3 4 1.30 3 3 2.06 3 4 2.60 Time profile in seconds ----------------------- 0.08: 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. 0.95: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.03: Set up l.s. refinement 0.00: Generate idealized H-atoms 2.02: Structure factors and derivatives 2.13: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.03: Apply other restraints 0.28: Solve l.s. equations 0.00: Generate HTAB table 0.05: Other dependent quantities, CIF, tables 0.13: Analysis of variance 0.03: Merge reflections for Fourier and .fcf 0.08: Fourier summations 0.03: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + s92 finished at 15:51:02 Total CPU time: 5.8 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++