+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2007src0399 started at 22:35:09 on 20-Mar-2007 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2007src0399 in Cc CELL 0.71073 14.6358 16.3497 12.3448 90.000 107.455 90.000 ZERR 4.00 0.0002 0.0002 0.0001 0.000 0.001 0.000 LATT -7 SYMM X, - Y, 1/2 + Z SFAC C H N O P CL UNIT 48 48 32 4 24 32 V = 2817.98 F(000) = 1496.0 Mu = 1.17 mm-1 Cell Wt = 3014.86 Rho = 1.777 MERG 2 OMIT -3.00 55.00 OMIT -2 0 2 FMAP 2 PLAN 20 SIZE 0.01 0.02 0.50 ACTA BOND WGHT 0.00000 3.13760 L.S. 4 TEMP -153.00 FVAR 0.30943 H4N 2 0.307670 0.455080 0.818621 11.00000 0.01893 H5N 2 0.127385 0.561655 1.167825 11.00000 0.04078 MOLE 1 C1 1 0.411799 0.514813 0.912899 11.00000 0.01238 0.01275 = 0.02029 0.00069 0.00590 0.00065 C2 1 0.456993 0.522468 0.829621 11.00000 0.01996 0.03247 = 0.01764 0.00133 0.00501 -0.00031 AFIX 43 H2 2 0.426804 0.502375 0.755260 11.00000 -1.20000 AFIX 0 C3 1 0.546118 0.559354 0.854493 11.00000 0.01869 0.03619 = 0.03044 0.00590 0.01245 -0.00229 AFIX 43 H3 2 0.576751 0.563982 0.796944 11.00000 -1.20000 AFIX 0 C4 1 0.591238 0.589617 0.962249 11.00000 0.01571 0.02001 = 0.04554 -0.00564 0.01094 -0.00572 AFIX 43 H4 2 0.652097 0.615334 0.978960 11.00000 -1.20000 AFIX 0 C5 1 0.545498 0.581465 1.044859 11.00000 0.01557 0.03352 = 0.03693 -0.01705 0.00620 -0.00412 AFIX 43 H5 2 0.575935 0.601649 1.119107 11.00000 -1.20000 AFIX 0 C6 1 0.456140 0.544496 1.022002 11.00000 0.01881 0.02966 = 0.02514 -0.01063 0.00871 -0.00681 AFIX 43 H6 2 0.425777 0.539533 1.079758 11.00000 -1.20000 AFIX 0 C7 1 0.015937 0.555508 1.036339 11.00000 0.01373 0.00952 = 0.01989 -0.00218 0.00414 -0.00145 C8 1 -0.016851 0.571618 0.920209 11.00000 0.01798 0.01470 = 0.02273 -0.00017 0.00388 -0.00046 AFIX 43 H8 2 0.026220 0.590082 0.881201 11.00000 -1.20000 AFIX 0 C9 1 -0.113784 0.560315 0.861754 11.00000 0.02077 0.01407 = 0.02562 -0.00069 -0.00222 0.00500 AFIX 43 H9 2 -0.136778 0.571151 0.782585 11.00000 -1.20000 AFIX 0 C10 1 -0.176309 0.533443 0.918655 11.00000 0.01040 0.02534 = 0.04199 -0.00658 0.00211 0.00027 AFIX 43 H10 2 -0.242091 0.525735 0.878445 11.00000 -1.20000 AFIX 0 C11 1 -0.143797 0.517915 1.032637 11.00000 0.01930 0.03729 = 0.04096 -0.00646 0.01652 -0.01056 AFIX 43 H11 2 -0.187360 0.499840 1.071196 11.00000 -1.20000 AFIX 0 C12 1 -0.047424 0.528321 1.092849 11.00000 0.02046 0.02927 = 0.01806 -0.00180 0.00565 -0.00523 AFIX 43 H12 2 -0.025201 0.516925 1.171904 11.00000 -1.20000 AFIX 0 N1 3 0.160114 0.300468 1.007283 11.00000 0.02604 0.01190 = 0.01761 0.00155 0.00403 -0.00655 N2 3 0.279181 0.430183 1.074329 11.00000 0.01760 0.01756 = 0.01331 0.00264 0.00215 -0.00238 N3 3 0.148709 0.429416 0.864827 11.00000 0.01304 0.01367 = 0.01167 -0.00102 0.00062 -0.00149 N4 3 0.321382 0.474885 0.883457 11.00000 0.01480 0.01600 = 0.01478 -0.00475 0.00435 -0.00365 N5 3 0.114267 0.565841 1.100454 11.00000 0.01499 0.01601 = 0.01322 0.00114 0.00484 -0.00046 N6 3 0.284343 0.631465 1.170598 11.00000 0.01335 0.01351 = 0.01267 0.00014 0.00033 0.00017 N7 3 0.277907 0.796744 1.138014 11.00000 0.02754 0.01103 = 0.01883 -0.00029 -0.00069 -0.00297 N8 3 0.149243 0.698830 0.991525 11.00000 0.01798 0.01406 = 0.01606 0.00019 0.00167 0.00002 O1 4 0.222533 0.564387 0.969087 11.00000 0.01792 0.00940 = 0.01568 -0.00002 0.00642 -0.00018 P1 5 0.105023 0.346288 0.894209 11.00000 0.01344 0.01198 = 0.01498 -0.00171 0.00421 -0.00285 P2 5 0.240020 0.345534 1.103487 11.00000 0.02023 0.01428 = 0.01276 0.00163 0.00355 -0.00067 P3 5 0.242233 0.469661 0.951409 11.00000 0.01240 0.01197 = 0.01184 -0.00029 0.00320 -0.00140 P4 5 0.193301 0.619221 1.061256 11.00000 0.01212 0.01090 = 0.01257 -0.00085 0.00295 -0.00113 P5 5 0.329478 0.719583 1.206699 11.00000 0.01473 0.01451 = 0.01533 -0.00179 0.00297 -0.00318 P6 5 0.190554 0.786819 1.025835 11.00000 0.02208 0.01089 = 0.01595 0.00031 0.00431 -0.00118 CL1 6 0.088976 0.268741 0.764435 11.00000 0.02030 0.01740 = 0.01773 -0.00527 0.00601 -0.00420 CL2 6 -0.030834 0.362755 0.890543 11.00000 0.01509 0.02241 = 0.03456 -0.00642 0.01137 -0.00380 CL3 6 0.193283 0.358856 1.238447 11.00000 0.05553 0.02937 = 0.02139 -0.00542 0.02130 -0.01507 CL4 6 0.347494 0.267078 1.161672 11.00000 0.03223 0.02989 = 0.04020 0.01348 -0.00120 0.01059 CL5 6 0.344248 0.735719 1.371205 11.00000 0.02861 0.01881 = 0.01530 -0.00320 0.00309 -0.00366 CL6 6 0.466148 0.721084 1.208369 11.00000 0.01841 0.03546 = 0.04260 -0.01108 0.01262 -0.00976 CL7 6 0.086566 0.862240 1.036555 11.00000 0.03653 0.01963 = 0.03137 0.00057 0.00841 0.01114 CL8 6 0.226169 0.836222 0.895613 11.00000 0.03725 0.02911 = 0.02206 0.00489 0.00907 -0.01233 HKLF 4 Covalent radii and connectivity table for 2007src0399 in Cc C 0.770 H 0.320 N 0.700 O 0.660 P 1.100 CL 0.990 C1 - C2 C6 N4 C2 - C1 C3 C3 - C2 C4 C4 - C5 C3 C5 - C4 C6 C6 - C5 C1 C7 - C12 C8 N5 C8 - C7 C9 C9 - C10 C8 C10 - C11 C9 C11 - C10 C12 C12 - C7 C11 N1 - P1 P2 N2 - P2 P3 N3 - P1 P3 N4 - C1 P3 N5 - C7 P4 N6 - P5 P4 N7 - P5 P6 N8 - P6 P4 O1 - P3 P4 P1 - N1 N3 Cl2 Cl1 P2 - N1 N2 Cl4 Cl3 P3 - N2 O1 N3 N4 P4 - N8 N6 O1 N5 P5 - N7 N6 Cl5 Cl6 P6 - N8 N7 Cl7 Cl8 Cl1 - P1 Cl2 - P1 Cl3 - P2 Cl4 - P2 Cl5 - P5 Cl6 - P5 Cl7 - P6 Cl8 - P6 Floating origin restraints generated 24343 Reflections read, of which 456 rejected -18 =< h =< 18, -21 =< k =< 21, -15 =< l =< 16, Max. 2-theta = 54.99 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) -6 16 1 12.18 1.01 3 5.85 2 10 9 20.83 2.73 6 16.38 2 Inconsistent equivalents 6203 Unique reflections, of which 0 suppressed R(int) = 0.0516 R(sigma) = 0.0578 Friedel opposites not merged Maximum memory for data reduction = 2401 / 74871 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 = 3214 / 409465 wR2 = 0.0677 before cycle 1 for 6203 data and 324 / 324 parameters GooF = S = 1.037; Restrained GooF = 1.036 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 3.14 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.30947 0.00028 0.140 OSF Mean shift/esd = 0.019 Maximum = 0.140 for OSF Max. shift = 0.002 A for H4N Max. dU = 0.000 for H4N Least-squares cycle 2 Maximum vector length = 511 Memory required = 3214 / 409465 wR2 = 0.0677 before cycle 2 for 6203 data and 324 / 324 parameters GooF = S = 1.037; Restrained GooF = 1.037 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 3.14 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.30948 0.00028 0.053 OSF Mean shift/esd = 0.007 Maximum = 0.053 for OSF Max. shift = 0.001 A for H4N Max. dU = 0.000 for H4N Least-squares cycle 3 Maximum vector length = 511 Memory required = 3214 / 409465 wR2 = 0.0677 before cycle 3 for 6203 data and 324 / 324 parameters GooF = S = 1.037; Restrained GooF = 1.037 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 3.14 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.30948 0.00028 0.002 OSF Mean shift/esd = 0.000 Maximum = -0.008 for z H4N Max. shift = 0.000 A for H4N Max. dU = 0.000 for H4N Least-squares cycle 4 Maximum vector length = 511 Memory required = 3214 / 409465 wR2 = 0.0677 before cycle 4 for 6203 data and 324 / 324 parameters GooF = S = 1.037; Restrained GooF = 1.037 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 3.14 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.30949 0.00028 0.002 OSF Mean shift/esd = 0.000 Maximum = -0.004 for z H4N Max. shift = 0.000 A for H4N Max. dU = 0.000 for H4N No correlation matrix elements larger than 0.500 Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2 0.4268 0.5024 0.7553 43 0.950 0.000 C2 C1 C3 H3 0.5767 0.5640 0.7969 43 0.950 0.000 C3 C2 C4 H4 0.6521 0.6153 0.9790 43 0.950 0.000 C4 C5 C3 H5 0.5759 0.6016 1.1191 43 0.950 0.000 C5 C4 C6 H6 0.4258 0.5395 1.0798 43 0.950 0.000 C6 C5 C1 H8 0.0262 0.5901 0.8812 43 0.950 0.000 C8 C7 C9 H9 -0.1368 0.5712 0.7826 43 0.950 0.000 C9 C10 C8 H10 -0.2421 0.5257 0.8785 43 0.950 0.000 C10 C11 C9 H11 -0.1874 0.4998 1.0712 43 0.950 0.000 C11 C10 C12 H12 -0.0252 0.5169 1.1719 43 0.950 0.000 C12 C7 C11 2007src0399 in Cc ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq H4N 0.30764 0.45516 0.81844 1.00000 0.01926 0.06837 0.00234 0.00207 0.00306 0.00000 0.00849 H5N 0.12731 0.56172 1.16768 1.00000 0.04062 0.07935 0.00289 0.00250 0.00341 0.00000 0.01185 C1 0.41180 0.51481 0.91289 1.00000 0.01239 0.01274 0.02033 0.00071 0.00592 0.00065 0.01493 0.00528 0.00019 0.00016 0.00023 0.00000 0.00131 0.00129 0.00145 0.00103 0.00104 0.00104 0.00055 C2 0.45700 0.52247 0.82964 1.00000 0.01993 0.03250 0.01766 0.00132 0.00497 -0.00027 0.02351 0.00608 0.00022 0.00020 0.00025 0.00000 0.00150 0.00170 0.00151 0.00123 0.00115 0.00127 0.00065 H2 0.42681 0.50238 0.75528 1.00000 0.02821 0.00000 0.00000 C3 0.54611 0.55936 0.85449 1.00000 0.01871 0.03621 0.03046 0.00591 0.01248 -0.00227 0.02734 0.00639 0.00022 0.00021 0.00028 0.00000 0.00151 0.00183 0.00174 0.00138 0.00127 0.00131 0.00069 H3 0.57673 0.56399 0.79693 1.00000 0.03280 0.00000 0.00000 C4 0.59123 0.58962 0.96225 1.00000 0.01571 0.02001 0.04549 -0.00563 0.01088 -0.00578 0.02669 0.00603 0.00022 0.00019 0.00029 0.00000 0.00148 0.00156 0.00202 0.00136 0.00131 0.00121 0.00069 H4 0.65210 0.61533 0.97896 1.00000 0.03203 0.00000 0.00000 C5 0.54550 0.58147 1.04485 1.00000 0.01556 0.03352 0.03690 -0.01703 0.00618 -0.00414 0.02903 0.00593 0.00022 0.00021 0.00030 0.00000 0.00150 0.00180 0.00191 0.00142 0.00130 0.00127 0.00074 H5 0.57593 0.60165 1.11910 1.00000 0.03484 0.00000 0.00000 C6 0.45615 0.54450 1.02200 1.00000 0.01878 0.02962 0.02522 -0.01064 0.00873 -0.00685 0.02407 0.00561 0.00021 0.00019 0.00027 0.00000 0.00152 0.00165 0.00162 0.00129 0.00120 0.00126 0.00065 H6 0.42579 0.53954 1.07976 1.00000 0.02888 0.00000 0.00000 C7 0.01593 0.55551 1.03634 1.00000 0.01375 0.00953 0.01990 -0.00221 0.00409 -0.00143 0.01460 0.00514 0.00020 0.00016 0.00023 0.00000 0.00126 0.00121 0.00143 0.00101 0.00103 0.00102 0.00053 C8 -0.01685 0.57162 0.92020 1.00000 0.01805 0.01470 0.02277 -0.00013 0.00395 -0.00050 0.01899 0.00542 0.00021 0.00017 0.00024 0.00000 0.00145 0.00137 0.00151 0.00112 0.00115 0.00113 0.00059 H8 0.02622 0.59008 0.88119 1.00000 0.02278 0.00000 0.00000 C9 -0.11379 0.56032 0.86176 1.00000 0.02080 0.01410 0.02561 -0.00073 -0.00220 0.00499 0.02218 0.00563 0.00021 0.00017 0.00027 0.00000 0.00154 0.00137 0.00161 0.00114 0.00121 0.00114 0.00065 H9 -0.13678 0.57116 0.78259 1.00000 0.02662 0.00000 0.00000 C10 -0.17631 0.53344 0.91866 1.00000 0.01041 0.02534 0.04198 -0.00655 0.00207 0.00028 0.02718 0.00599 0.00022 0.00019 0.00029 0.00000 0.00138 0.00165 0.00200 0.00135 0.00125 0.00119 0.00072 H10 -0.24209 0.52574 0.87845 1.00000 0.03262 0.00000 0.00000 C11 -0.14381 0.51791 1.03261 1.00000 0.01940 0.03726 0.04101 -0.00651 0.01662 -0.01058 0.03090 0.00642 0.00023 0.00021 0.00031 0.00000 0.00165 0.00189 0.00201 0.00153 0.00144 0.00139 0.00075 H11 -0.18737 0.49983 1.07116 1.00000 0.03708 0.00000 0.00000 C12 -0.04742 0.52832 1.09284 1.00000 0.02041 0.02927 0.01801 -0.00178 0.00557 -0.00517 0.02261 0.00572 0.00022 0.00019 0.00025 0.00000 0.00148 0.00168 0.00153 0.00119 0.00116 0.00124 0.00064 H12 -0.02520 0.51693 1.17189 1.00000 0.02713 0.00000 0.00000 N1 0.16011 0.30047 1.00728 1.00000 0.02608 0.01188 0.01766 0.00153 0.00405 -0.00658 0.01909 0.00455 0.00018 0.00014 0.00020 0.00000 0.00133 0.00112 0.00121 0.00093 0.00097 0.00098 0.00051 N2 0.27918 0.43019 1.07433 1.00000 0.01758 0.01759 0.01329 0.00259 0.00211 -0.00233 0.01671 0.00438 0.00017 0.00014 0.00019 0.00000 0.00123 0.00120 0.00114 0.00088 0.00091 0.00095 0.00049 N3 0.14872 0.42941 0.86483 1.00000 0.01305 0.01365 0.01171 -0.00102 0.00064 -0.00146 0.01348 0.00409 0.00016 0.00013 0.00018 0.00000 0.00109 0.00110 0.00111 0.00084 0.00085 0.00088 0.00045 N4 0.32139 0.47488 0.88346 1.00000 0.01477 0.01597 0.01484 -0.00473 0.00436 -0.00363 0.01521 0.00456 0.00016 0.00014 0.00021 0.00000 0.00119 0.00117 0.00120 0.00094 0.00091 0.00091 0.00047 N5 0.11427 0.56584 1.10045 1.00000 0.01500 0.01602 0.01318 0.00112 0.00482 -0.00047 0.01460 0.00457 0.00016 0.00014 0.00021 0.00000 0.00117 0.00117 0.00123 0.00090 0.00092 0.00090 0.00047 N6 0.28434 0.63146 1.17060 1.00000 0.01342 0.01349 0.01265 0.00014 0.00033 0.00019 0.01397 0.00424 0.00016 0.00014 0.00018 0.00000 0.00113 0.00110 0.00111 0.00082 0.00085 0.00086 0.00046 N7 0.27791 0.79674 1.13802 1.00000 0.02759 0.01108 0.01877 -0.00027 -0.00070 -0.00299 0.02083 0.00456 0.00019 0.00014 0.00021 0.00000 0.00136 0.00115 0.00124 0.00091 0.00097 0.00096 0.00052 N8 0.14925 0.69883 0.99153 1.00000 0.01801 0.01411 0.01601 0.00019 0.00167 -0.00002 0.01680 0.00440 0.00017 0.00014 0.00019 0.00000 0.00119 0.00111 0.00117 0.00090 0.00091 0.00092 0.00048 O1 0.22254 0.56439 0.96909 1.00000 0.01790 0.00942 0.01567 -0.00001 0.00642 -0.00018 0.01403 0.00363 0.00014 0.00011 0.00016 0.00000 0.00094 0.00084 0.00095 0.00070 0.00073 0.00075 0.00037 P1 0.10502 0.34629 0.89421 1.00000 0.01347 0.01200 0.01499 -0.00170 0.00422 -0.00284 0.01350 0.00127 0.00005 0.00004 0.00006 0.00000 0.00033 0.00033 0.00035 0.00025 0.00026 0.00026 0.00014 P2 0.24002 0.34554 1.10349 1.00000 0.02024 0.01430 0.01277 0.00164 0.00355 -0.00068 0.01608 0.00138 0.00005 0.00004 0.00006 0.00000 0.00036 0.00033 0.00033 0.00026 0.00026 0.00028 0.00015 P3 0.24224 0.46966 0.95141 1.00000 0.01244 0.01198 0.01187 -0.00028 0.00321 -0.00139 0.01219 0.00127 0.00005 0.00004 0.00006 0.00000 0.00032 0.00032 0.00032 0.00025 0.00024 0.00025 0.00014 P4 0.19330 0.61922 1.06126 1.00000 0.01213 0.01093 0.01257 -0.00085 0.00295 -0.00114 0.01204 0.00127 0.00005 0.00004 0.00006 0.00000 0.00032 0.00031 0.00032 0.00025 0.00025 0.00025 0.00014 P5 0.32948 0.71958 1.20670 1.00000 0.01475 0.01452 0.01533 -0.00180 0.00297 -0.00318 0.01521 0.00134 0.00005 0.00004 0.00006 0.00000 0.00034 0.00034 0.00034 0.00025 0.00026 0.00027 0.00015 P6 0.19055 0.78682 1.02583 1.00000 0.02210 0.01091 0.01596 0.00031 0.00432 -0.00116 0.01663 0.00135 0.00005 0.00004 0.00006 0.00000 0.00038 0.00032 0.00036 0.00026 0.00028 0.00028 0.00015 Cl1 0.08898 0.26874 0.76444 1.00000 0.02032 0.01740 0.01775 -0.00528 0.00602 -0.00420 0.01842 0.00128 0.00005 0.00004 0.00006 0.00000 0.00033 0.00034 0.00032 0.00026 0.00025 0.00026 0.00014 Cl2 -0.03083 0.36276 0.89055 1.00000 0.01510 0.02241 0.03457 -0.00642 0.01136 -0.00380 0.02317 0.00134 0.00005 0.00004 0.00006 0.00000 0.00033 0.00036 0.00042 0.00029 0.00029 0.00027 0.00016 Cl3 0.19328 0.35885 1.23845 1.00000 0.05554 0.02937 0.02142 -0.00542 0.02131 -0.01506 0.03330 0.00164 0.00007 0.00005 0.00007 0.00000 0.00057 0.00043 0.00038 0.00031 0.00036 0.00037 0.00020 Cl4 0.34749 0.26708 1.16167 1.00000 0.03224 0.02989 0.04022 0.01348 -0.00119 0.01060 0.03677 0.00175 0.00006 0.00005 0.00007 0.00000 0.00045 0.00042 0.00050 0.00035 0.00036 0.00035 0.00021 Cl5 0.34425 0.73572 1.37120 1.00000 0.02862 0.01882 0.01530 -0.00319 0.00309 -0.00366 0.02168 0.00129 0.00005 0.00004 0.00006 0.00000 0.00039 0.00034 0.00034 0.00026 0.00027 0.00028 0.00015 Cl6 0.46615 0.72108 1.20837 1.00000 0.01844 0.03548 0.04261 -0.01107 0.01263 -0.00977 0.03141 0.00151 0.00006 0.00005 0.00007 0.00000 0.00037 0.00045 0.00047 0.00035 0.00032 0.00031 0.00019 Cl7 0.08657 0.86224 1.03656 1.00000 0.03655 0.01964 0.03139 0.00056 0.00841 0.01111 0.02958 0.00161 0.00006 0.00005 0.00007 0.00000 0.00045 0.00036 0.00042 0.00029 0.00033 0.00032 0.00018 Cl8 0.22617 0.83622 0.89562 1.00000 0.03726 0.02912 0.02207 0.00489 0.00907 -0.01233 0.02944 0.00151 0.00006 0.00005 0.00006 0.00000 0.00045 0.00041 0.00038 0.00031 0.00031 0.00034 0.00018 Final Structure Factor Calculation for 2007src0399 in Cc Total number of l.s. parameters = 324 Maximum vector length = 511 Memory required = 2892 / 27090 wR2 = 0.0677 before cycle 5 for 6203 data and 2 / 324 parameters GooF = S = 1.037; Restrained GooF = 1.037 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 3.14 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0303 for 5903 Fo > 4sig(Fo) and 0.0333 for all 6203 data wR2 = 0.0677, GooF = S = 1.037, Restrained GooF = 1.037 for all data Flack x parameter = 0.2375 with esd 0.0483 Expected values are 0 (within 3 esd's) for correct and +1 for inverted absolute structure. Note that this rough estimate ignores correlation with other parameters; if the above value differs significantly from zero, it is ESSENTIAL to test the inverted structure or refine x as a full-matrix parameter using TWIN and BASF ** Possible racemic twin or wrong absolute structure - try TWIN refinement ** Occupancy sum of asymmetric unit = 35.00 for non-hydrogen and 12.00 for hydrogen atoms Principal mean square atomic displacements U 0.0204 0.0129 0.0115 C1 0.0327 0.0204 0.0175 C2 0.0400 0.0288 0.0132 C3 0.0468 0.0219 0.0114 C4 0.0529 0.0200 0.0143 C5 0.0389 0.0181 0.0152 C6 0.0208 0.0141 0.0088 C7 0.0246 0.0178 0.0146 C8 0.0375 0.0179 0.0111 C9 0.0480 0.0232 0.0104 C10 0.0484 0.0332 0.0111 C11 0.0316 0.0187 0.0175 C12 0.0309 0.0175 0.0089 N1 0.0228 0.0153 0.0120 N2 0.0169 0.0141 0.0094 N3 0.0207 0.0149 0.0101 N4 0.0166 0.0150 0.0122 N5 0.0182 0.0135 0.0103 N6 0.0356 0.0164 0.0104 N7 0.0221 0.0143 0.0140 N8 0.0182 0.0144 0.0094 O1 0.0161 0.0146 0.0097 P1 0.0214 0.0151 0.0117 P2 0.0138 0.0120 0.0108 P3 0.0135 0.0127 0.0100 P4 0.0180 0.0167 0.0109 P5 0.0232 0.0159 0.0108 P6 0.0243 0.0189 0.0120 Cl1 0.0375 0.0199 0.0122 Cl2 0.0629 0.0227 0.0143 Cl3 0.0553 0.0416 0.0134 Cl4 0.0316 0.0205 0.0130 Cl5 0.0511 0.0296 0.0135 Cl6 0.0433 0.0314 0.0140 Cl7 0.0482 0.0259 0.0143 Cl8 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.052 0.079 0.102 0.121 0.143 0.168 0.199 0.236 0.308 1.000 Number in group 636. 620. 634. 592. 617. 643. 604. 622. 610. 625. GooF 1.054 1.068 1.051 1.053 1.068 1.086 0.986 1.049 0.985 0.954 K 0.997 0.979 0.983 0.987 0.996 1.008 1.014 1.013 1.012 0.990 Resolution(A) 0.77 0.80 0.83 0.87 0.92 0.98 1.05 1.16 1.33 1.67 inf Number in group 647. 607. 615. 610. 622. 627. 613. 624. 613. 625. GooF 1.011 0.998 1.052 1.073 1.086 0.994 0.962 0.895 0.923 1.310 K 0.988 1.034 1.027 1.015 1.007 0.999 0.998 1.006 1.005 0.983 R1 0.072 0.059 0.053 0.045 0.039 0.033 0.025 0.018 0.016 0.021 Recommended weighting scheme: WGHT 0.0000 3.1530 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) -7 15 0 3746.39 5218.82 5.81 0.230 0.96 7 15 0 3494.01 5233.22 5.54 0.230 0.96 -1 1 2 3041.60 4258.24 5.19 0.208 5.73 -6 16 -1 1589.11 2397.62 5.08 0.156 0.92 -9 1 13 5368.42 7568.04 4.84 0.277 0.91 5 3 3 595.58 361.75 4.79 0.061 1.88 -3 5 14 609.98 1196.91 4.44 0.110 0.85 0 0 -2 25647.64 36219.98 4.40 0.605 5.89 -4 2 -4 672.24 453.26 4.37 0.068 1.92 -5 3 -3 603.77 401.12 4.37 0.064 1.88 4 2 4 662.08 437.17 4.25 0.067 1.92 2 4 5 1907.08 1527.53 4.00 0.124 1.83 -5 5 -1 198.58 77.44 4.00 0.028 2.01 -3 11 11 419.23 893.21 3.99 0.095 0.89 -11 7 8 1501.82 2275.42 3.96 0.152 1.03 5 5 1 156.28 57.34 3.92 0.024 2.01 5 5 13 873.87 1534.01 3.69 0.125 0.77 3 3 -5 143.93 54.83 3.67 0.024 2.21 5 5 11 862.52 1254.44 3.67 0.113 0.88 9 5 9 441.63 772.81 3.62 0.088 0.85 -6 0 0 1096.27 734.77 3.60 0.086 2.33 0 2 2 59013.84 68445.30 3.59 0.832 4.78 -11 9 6 1795.40 2518.87 3.47 0.160 1.03 2 8 0 2913.29 2434.00 3.47 0.157 1.96 3 5 -4 931.45 717.56 3.45 0.085 2.18 -1 17 -2 1351.40 1907.24 3.42 0.139 0.94 -1 3 7 4258.46 3685.87 3.40 0.193 1.65 -12 6 14 -91.88 167.29 3.36 0.041 0.77 -3 1 -5 1646.29 1370.28 3.35 0.118 1.87 -6 10 13 2490.57 1581.97 3.30 0.127 0.82 2 4 3 2870.48 2481.92 3.22 0.158 2.45 1 7 14 293.16 590.52 3.20 0.077 0.78 -11 11 2 167.30 412.60 3.19 0.065 0.99 -10 4 13 120.78 260.80 3.18 0.051 0.87 6 0 0 1122.98 685.62 3.18 0.083 2.33 -4 4 -3 1940.18 1617.43 3.15 0.128 2.00 5 19 4 753.30 1138.72 3.08 0.107 0.77 15 3 -12 221.84 405.52 3.08 0.064 0.80 5 1 12 655.24 1237.41 3.07 0.112 0.85 2 18 -4 2360.65 2928.05 3.05 0.172 0.87 -3 15 0 6069.93 7002.12 3.04 0.266 1.06 -6 0 -2 8663.37 9708.03 3.03 0.313 1.97 -15 1 -2 92.44 231.12 3.02 0.048 0.88 -4 10 12 1105.28 1470.21 3.00 0.122 0.87 -9 9 5 4454.11 5044.77 2.94 0.226 1.17 -1 5 4 1504.66 1816.06 2.92 0.136 2.24 1 3 -7 4405.62 3774.65 2.91 0.195 1.65 -10 6 13 760.25 1028.23 2.90 0.102 0.85 -2 8 0 2940.89 2485.70 2.90 0.159 1.96 0 8 0 5762.78 6542.06 2.90 0.257 2.04 Bond lengths and angles C1 - Distance Angles C2 1.3847 (0.0041) C6 1.3952 (0.0040) 119.84 (0.27) N4 1.4216 (0.0035) 117.85 (0.25) 122.30 (0.26) C1 - C2 C6 C2 - Distance Angles C1 1.3847 (0.0041) C3 1.3851 (0.0043) 120.18 (0.28) C2 - C1 C3 - Distance Angles C2 1.3851 (0.0043) C4 1.3869 (0.0046) 120.90 (0.29) C3 - C2 C4 - Distance Angles C5 1.3839 (0.0048) C3 1.3869 (0.0046) 118.42 (0.28) C4 - C5 C5 - Distance Angles C4 1.3839 (0.0048) C6 1.3905 (0.0043) 121.71 (0.30) C5 - C4 C6 - Distance Angles C5 1.3905 (0.0043) C1 1.3952 (0.0040) 118.95 (0.30) C6 - C5 C7 - Distance Angles C12 1.3899 (0.0041) C8 1.3937 (0.0039) 120.06 (0.26) N5 1.4294 (0.0035) 118.20 (0.25) 121.74 (0.26) C7 - C12 C8 C8 - Distance Angles C7 1.3937 (0.0039) C9 1.3976 (0.0040) 119.28 (0.28) C8 - C7 C9 - Distance Angles C10 1.3819 (0.0048) C8 1.3976 (0.0040) 120.27 (0.29) C9 - C10 C10 - Distance Angles C11 1.3668 (0.0051) C9 1.3819 (0.0048) 120.21 (0.28) C10 - C11 C11 - Distance Angles C10 1.3668 (0.0051) C12 1.3938 (0.0043) 120.69 (0.30) C11 - C10 C12 - Distance Angles C7 1.3899 (0.0041) C11 1.3938 (0.0043) 119.49 (0.29) C12 - C7 N1 - Distance Angles P1 1.5763 (0.0024) P2 1.5773 (0.0024) 120.77 (0.14) N1 - P1 N2 - Distance Angles P2 1.5803 (0.0024) P3 1.5872 (0.0023) 122.08 (0.15) N2 - P2 N3 - Distance Angles P1 1.5896 (0.0023) P3 1.6035 (0.0022) 121.35 (0.14) N3 - P1 N4 - Distance Angles C1 1.4216 (0.0035) P3 1.6235 (0.0024) 130.23 (0.20) N4 - C1 N5 - Distance Angles C7 1.4294 (0.0035) P4 1.6338 (0.0024) 125.72 (0.20) N5 - C7 N6 - Distance Angles P5 1.5920 (0.0023) P4 1.5995 (0.0022) 121.34 (0.14) N6 - P5 N7 - Distance Angles P5 1.5799 (0.0024) P6 1.5864 (0.0024) 121.13 (0.15) N7 - P5 N8 - Distance Angles P6 1.5687 (0.0023) P4 1.5867 (0.0023) 123.01 (0.15) N8 - P6 O1 - Distance Angles P3 1.6022 (0.0019) P4 1.6043 (0.0020) 137.22 (0.13) O1 - P3 P1 - Distance Angles N1 1.5763 (0.0024) N3 1.5896 (0.0023) 118.32 (0.12) Cl2 1.9935 (0.0010) 109.03 (0.10) 110.25 (0.09) Cl1 2.0009 (0.0010) 108.29 (0.10) 108.53 (0.09) 101.00 (0.04) P1 - N1 N3 Cl2 P2 - Distance Angles N1 1.5773 (0.0024) N2 1.5803 (0.0024) 118.38 (0.12) Cl4 1.9894 (0.0011) 107.34 (0.10) 110.21 (0.10) Cl3 1.9936 (0.0011) 108.51 (0.10) 109.48 (0.10) 101.59 (0.05) P2 - N1 N2 Cl4 P3 - Distance Angles N2 1.5872 (0.0023) O1 1.6022 (0.0019) 106.65 (0.12) N3 1.6035 (0.0022) 116.63 (0.12) 109.57 (0.11) N4 1.6235 (0.0024) 115.09 (0.13) 101.83 (0.11) 106.02 (0.12) P3 - N2 O1 N3 P4 - Distance Angles N8 1.5867 (0.0023) N6 1.5995 (0.0023) 117.08 (0.12) O1 1.6043 (0.0020) 103.01 (0.12) 109.66 (0.12) N5 1.6338 (0.0024) 112.97 (0.13) 107.54 (0.12) 105.94 (0.11) P4 - N8 N6 O1 P5 - Distance Angles N7 1.5799 (0.0024) N6 1.5920 (0.0023) 118.76 (0.13) Cl5 1.9943 (0.0010) 109.22 (0.10) 108.30 (0.09) Cl6 1.9943 (0.0010) 108.18 (0.11) 110.17 (0.09) 100.71 (0.04) P5 - N7 N6 Cl5 P6 - Distance Angles N8 1.5687 (0.0023) N7 1.5864 (0.0025) 118.28 (0.12) Cl7 1.9938 (0.0011) 110.18 (0.10) 108.07 (0.10) Cl8 2.0027 (0.0010) 108.98 (0.10) 108.90 (0.11) 101.04 (0.05) P6 - N8 N7 Cl7 Cl1 - Distance Angles P1 2.0009 (0.0010) Cl1 - Cl2 - Distance Angles P1 1.9935 (0.0010) Cl2 - Cl3 - Distance Angles P2 1.9936 (0.0011) Cl3 - Cl4 - Distance Angles P2 1.9894 (0.0011) Cl4 - Cl5 - Distance Angles P5 1.9943 (0.0010) Cl5 - Cl6 - Distance Angles P5 1.9943 (0.0010) Cl6 - Cl7 - Distance Angles P6 1.9938 (0.0011) Cl7 - Cl8 - Distance Angles P6 2.0027 (0.0010) Cl8 - FMAP and GRID set by program FMAP 2 1 37 GRID -1.471 -1 -2 1.471 1 2 R1 = 0.0268 for 3234 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.35 at 0.4005 0.2817 0.7123 [ 0.98 A from CL6 ] Deepest hole -0.40 at 0.3662 0.2513 0.1165 [ 0.74 A from CL4 ] Mean = 0.00, Rms deviation from mean = 0.07 e/A^3, Highest memory used = 3142 / 47640 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.4005 0.7183 1.2123 1.00000 0.05 0.35 0.98 CL6 1.02 P5 2.16 N6 2.17 N7 Q2 1 0.3493 0.2900 1.2211 1.00000 0.05 0.32 0.82 CL4 2.02 P2 2.61 CL3 2.91 N2 Q3 1 0.0001 0.5986 1.2447 1.00000 0.05 0.32 1.59 H12 2.08 CL2 2.13 C12 2.21 P1 Q4 1 0.3843 0.2838 1.1429 1.00000 0.05 0.30 0.70 CL4 2.26 P2 2.83 N2 3.04 CL1 Q5 1 0.2098 0.7177 1.2381 1.00000 0.05 0.28 1.90 P5 1.90 CL1 2.10 N6 2.17 CL5 Q6 1 0.4434 0.5279 0.8786 1.00000 0.05 0.28 0.70 C2 0.75 C1 1.53 H2 1.70 C3 Q7 1 -0.1341 0.3901 0.7174 1.00000 0.05 0.27 2.26 CL2 2.39 H12 2.50 H11 2.63 C12 Q8 1 0.0344 0.2177 0.8387 1.00000 0.05 0.27 1.62 CL1 2.35 P1 2.58 C4 2.60 C3 Q9 1 -0.0613 0.3611 0.7106 1.00000 0.05 0.27 2.13 CL2 2.15 H12 2.37 C12 2.46 CL4 Q10 1 0.1132 0.4532 0.9648 1.00000 0.05 0.27 1.53 N3 1.94 P1 1.96 P3 2.41 O1 Q11 1 0.1006 0.7023 0.9766 1.00000 0.05 0.27 0.68 N8 1.88 P6 1.98 P4 2.27 H8 Q12 1 0.3862 0.6395 1.0991 1.00000 0.05 0.26 1.77 H6 1.95 N6 2.00 CL6 2.20 P5 Q13 1 0.1613 0.3387 0.7423 1.00000 0.05 0.26 1.64 CL1 1.86 H5N 2.17 N3 2.27 P1 Q14 1 0.0424 0.3393 0.8985 1.00000 0.05 0.26 0.94 P1 1.11 CL2 1.95 N1 2.27 N3 Q15 1 0.1270 0.8143 1.0490 1.00000 0.05 0.26 0.97 CL7 1.14 P6 2.08 N8 2.17 N7 Q16 1 0.4456 0.4478 0.7809 1.00000 0.05 0.25 0.96 H2 1.35 C2 2.14 C1 2.21 H4N Q17 1 0.1430 0.4176 1.1092 1.00000 0.05 0.25 1.82 CL3 1.86 P2 2.17 N2 2.35 N1 Q18 1 -0.0087 0.3434 0.6848 1.00000 0.05 0.25 1.91 CL1 2.30 H12 2.37 C12 2.57 C7 Q19 1 0.4154 0.5806 1.0763 1.00000 0.05 0.25 0.69 H6 1.18 C6 2.05 C5 2.27 C1 Q20 1 0.2064 0.4212 0.8852 1.00000 0.05 0.25 0.82 N3 1.15 P3 1.90 N4 1.95 P1 Shortest distances between peaks (including symmetry equivalents) 9 18 0.96 3 9 1.09 12 19 1.12 5 13 1.17 3 18 1.19 7 9 1.19 2 4 1.23 6 16 1.79 10 17 1.80 1 12 1.86 3 7 1.90 10 20 1.97 11 15 2.02 3 14 2.08 8 14 2.11 7 18 2.14 13 20 2.16 10 14 2.17 13 18 2.37 9 14 2.39 16 19 2.47 14 18 2.52 4 9 2.56 4 18 2.56 12 16 2.58 3 13 2.58 2 8 2.67 6 19 2.73 4 8 2.74 8 18 2.74 5 15 2.78 14 20 2.79 2 9 2.82 3 10 2.85 1 19 2.85 1 16 2.86 14 17 2.88 1 5 2.90 5 20 2.92 8 9 2.94 2 7 2.96 13 14 2.96 7 14 2.98 Time profile in seconds ----------------------- 0.05: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.01: Generate connectivity array 0.01: Analyse DFIX/DANG restraints 0.00: Analyse SAME/SADI restraints 0.00: Generate CHIV restraints 0.00: Check if bonds in residues restrained 0.00: Generate DELU restraints 0.00: Generate SIMU restraints 0.00: Generate ISOR restraints 0.00: Generate NCSY restraints 0.01: Analyse other restraints etc. 3.45: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.02: OSF, H-atoms from difference map 0.02: Set up l.s. refinement 0.00: Generate idealized H-atoms 2.79: Structure factors and derivatives 6.23: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.06: Apply other restraints 0.65: Solve l.s. equations 0.00: Generate HTAB table 0.02: Other dependent quantities, CIF, tables 0.18: Analysis of variance 0.07: Merge reflections for Fourier and .fcf 0.14: Fourier summations 0.07: Peaksearch 0.01: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2007src0399 finished at 22:35:26 Total CPU time: 13.9 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++