+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + p-1 started at 15:57:09 on 22-Nov-2006 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL P-1 in P-1 CELL 0.71073 8.8804 14.1275 14.1255 91.749 107.376 107.382 ZERR 2.00 0.0002 0.0004 0.0003 0.002 0.002 0.001 LATT 1 SFAC C H N O P S NI UNIT 56 66 6 10 4 8 2 V = 1600.04 F(000) = 768.0 Mu = 1.01 mm-1 Cell Wt = 1480.93 Rho = 1.537 MERG 2 OMIT -3.00 55.00 OMIT 0 -1 1 OMIT 0 1 0 OMIT 0 0 1 OMIT 0 1 1 OMIT 0 -8 10 EQIV $1 -x-1, -y+1, -z-1 EQIV $2 -x-2, -y+1, -z-1 FREE C1S C1S_$1 FREE C2S C2S_$2 FREE N2 N2A FREE N2 C14A FREE C14 N2A FREE C14 C14A FREE C14 O2S FREE C14A O1S FREE O1S O2S FREE C14 H2AN FREE C14A H2N FMAP 2 PLAN 5 ACTA SIZE 0.23 0.12 0.07 BOND L.S. 6 TEMP -153.00 WGHT 0.0386 1.2005 EXTI 0.002113 FVAR 0.58270 MOLE 1 C1 1 -1.907289 0.087035 -0.695795 11.00000 0.02983 0.03227 = 0.02590 0.00116 0.00504 0.01290 C2 1 -1.957521 0.126551 -0.784934 11.00000 0.03794 0.03673 = 0.03632 0.00993 0.00652 0.01055 AFIX 43 H2 2 -1.878816 0.178693 -0.802696 11.00000 -1.20000 AFIX 0 C3 1 -2.119384 0.090655 -0.846873 11.00000 0.04146 0.04578 = 0.03571 0.01114 0.00258 0.01609 AFIX 43 H3 2 -2.152271 0.118633 -0.906923 11.00000 -1.20000 AFIX 0 C4 1 -2.235738 0.013894 -0.822821 11.00000 0.03041 0.03759 = 0.02734 -0.00391 0.00018 0.01414 C5 1 -2.189152 -0.026387 -0.735164 11.00000 0.03321 0.04466 = 0.02933 0.00293 0.01120 0.01273 AFIX 43 H5 2 -2.268370 -0.079048 -0.718362 11.00000 -1.20000 AFIX 0 C6 1 -2.024759 0.010919 -0.671497 11.00000 0.03376 0.04318 = 0.02599 0.00531 0.00473 0.01557 AFIX 43 H6 2 -1.992722 -0.016088 -0.610720 11.00000 -1.20000 AFIX 0 C7 1 -2.512631 -0.101933 -0.877742 11.00000 0.03077 0.05393 = 0.04377 -0.00997 0.00788 0.00955 AFIX 137 H7A 2 -2.469310 -0.158430 -0.871878 11.00000 -1.50000 H7B 2 -2.614798 -0.118673 -0.935353 11.00000 -1.50000 H7C 2 -2.537310 -0.087837 -0.816670 11.00000 -1.50000 AFIX 0 C8 1 -1.456330 0.294097 -0.607881 11.00000 0.04897 0.04262 = 0.07457 0.00832 0.00271 -0.00317 AFIX 137 H8A 2 -1.410027 0.293995 -0.535632 11.00000 -1.50000 H8B 2 -1.440304 0.363149 -0.622367 11.00000 -1.50000 H8C 2 -1.399299 0.263046 -0.642768 11.00000 -1.50000 AFIX 0 C9 1 -1.224911 0.181612 -0.370127 11.00000 0.03683 0.04135 = 0.03740 -0.00819 0.00337 0.00782 AFIX 43 H9 2 -1.294682 0.169457 -0.329271 11.00000 -1.20000 AFIX 0 C10 1 -1.077715 0.259214 -0.337417 11.00000 0.04261 0.05023 = 0.05264 -0.01321 -0.00308 0.00290 AFIX 43 H10 2 -1.047454 0.299038 -0.275065 11.00000 -1.20000 AFIX 0 C11 1 -0.974200 0.279510 -0.394297 11.00000 0.02762 0.05338 = 0.08409 -0.01462 -0.00107 0.00119 C12 1 -1.024309 0.219447 -0.484940 11.00000 0.03347 0.04819 = 0.08427 0.01169 0.02605 0.01030 AFIX 43 H12 2 -0.956452 0.230902 -0.526944 11.00000 -1.20000 AFIX 0 C13 1 -1.175498 0.142261 -0.513155 11.00000 0.03065 0.04028 = 0.04603 0.00414 0.01082 0.01121 AFIX 43 H13 2 -1.209375 0.101938 -0.575645 11.00000 -1.20000 AFIX 0 C14 1 -0.685883 0.374524 -0.373146 10.50000 0.04936 AFIX 13 H14 2 -0.697923 0.314051 -0.417088 10.50000 -1.20000 AFIX 0 C14A 1 -0.812184 0.374082 -0.373280 10.50000 0.04839 AFIX 13 H14A 2 -0.799200 0.417929 -0.312493 10.50000 -1.20000 AFIX 0 C15 1 -0.526025 0.394055 -0.279562 11.00000 0.02865 0.08646 = 0.05020 -0.01693 0.00266 -0.00072 C16 1 -0.421399 0.337317 -0.260089 11.00000 0.03947 0.05522 = 0.05020 -0.01485 0.00283 -0.00346 AFIX 43 H16 2 -0.450106 0.275685 -0.300758 11.00000 -1.20000 AFIX 0 C17 1 -0.274925 0.370359 -0.181361 11.00000 0.03603 0.03652 = 0.04272 -0.00812 0.00822 0.00082 AFIX 43 H17 2 -0.205692 0.329203 -0.168289 11.00000 -1.20000 AFIX 0 C18 1 -0.324721 0.513604 -0.142022 11.00000 0.03101 0.04385 = 0.04120 0.00449 0.01365 0.00873 AFIX 43 H18 2 -0.291609 0.575787 -0.101330 11.00000 -1.20000 AFIX 0 C19 1 -0.475294 0.485070 -0.219694 11.00000 0.03308 0.08500 = 0.04956 0.01137 0.01271 0.02451 AFIX 43 H19 2 -0.542804 0.527265 -0.231754 11.00000 -1.20000 AFIX 0 C20 1 -0.407055 0.304508 0.086906 11.00000 0.03211 0.02766 = 0.03087 -0.00005 0.01349 0.00439 C21 1 -0.457309 0.215264 0.126695 11.00000 0.03881 0.03790 = 0.03727 0.01011 0.01332 0.00658 AFIX 43 H21 2 -0.378842 0.197567 0.179046 11.00000 -1.20000 AFIX 0 C22 1 -0.619406 0.153374 0.090315 11.00000 0.04127 0.03540 = 0.04302 0.01392 0.01585 0.00189 AFIX 43 H22 2 -0.652046 0.093117 0.118019 11.00000 -1.20000 AFIX 0 C23 1 -0.736161 0.177066 0.014076 11.00000 0.02895 0.03104 = 0.03883 -0.00260 0.01602 -0.00005 C24 1 -0.689704 0.264959 -0.026494 11.00000 0.03221 0.03166 = 0.04154 0.00166 0.01177 0.00880 AFIX 43 H24 2 -0.768897 0.281910 -0.079037 11.00000 -1.20000 AFIX 0 C25 1 -0.524899 0.328260 0.010919 11.00000 0.03587 0.02733 = 0.04438 0.00586 0.01808 0.00660 AFIX 43 H25 2 -0.492827 0.388908 -0.016280 11.00000 -1.20000 AFIX 0 C26 1 -1.013270 0.122397 -0.102140 11.00000 0.02958 0.04346 = 0.05233 -0.01140 0.01040 0.00585 AFIX 137 H26A 2 -1.038890 0.182991 -0.087583 11.00000 -1.50000 H26B 2 -1.114965 0.064412 -0.119369 11.00000 -1.50000 H26C 2 -0.969586 0.129196 -0.158501 11.00000 -1.50000 AFIX 0 C27 1 0.043597 0.391540 0.293949 11.00000 0.04646 0.07194 = 0.04340 0.00855 -0.00625 0.00028 AFIX 137 H27A 2 0.100668 0.357904 0.261601 11.00000 -1.50000 H27B 2 0.059515 0.375041 0.362376 11.00000 -1.50000 H27C 2 0.089948 0.464085 0.295791 11.00000 -1.50000 AFIX 0 N1 3 -1.275615 0.121730 -0.457252 11.00000 0.02697 0.03265 = 0.03023 -0.00206 0.00388 0.00862 N2 3 -0.817675 0.350692 -0.332661 10.50000 0.06135 AFIX 3 H2N 2 -0.806177 0.378448 -0.273199 10.50000 -1.20000 AFIX 0 N2A 3 -0.683104 0.332584 -0.351623 10.50000 0.05922 AFIX 3 H2AN 2 -0.695999 0.273188 -0.380192 10.50000 -1.20000 AFIX 0 N3 3 -0.223996 0.457473 -0.121831 11.00000 0.02481 0.03019 = 0.03377 -0.00154 0.00783 0.00268 O1 4 -2.391984 -0.016508 -0.891210 11.00000 0.03088 0.05090 = 0.04007 0.00131 -0.00324 0.01284 O2 4 -1.633014 0.237998 -0.641742 11.00000 0.04415 0.03213 = 0.04584 0.00349 0.00253 0.00536 O3 4 -0.892405 0.108801 -0.016824 11.00000 0.03272 0.03962 = 0.04913 0.00217 0.01319 -0.00261 O4 4 -0.132611 0.358451 0.237956 11.00000 0.04293 0.04799 = 0.03210 0.00700 0.00708 0.00479 P1 5 -1.691586 0.124039 -0.621317 11.00000 0.02999 0.03163 = 0.02782 0.00083 0.00380 0.00919 P2 5 -0.191650 0.378818 0.123960 11.00000 0.02978 0.02804 = 0.03205 0.00117 0.00945 0.00302 S1 6 -1.569562 0.045925 -0.670360 11.00000 0.03154 0.04389 = 0.02463 0.00146 0.00593 0.01282 S2 6 -1.659150 0.112736 -0.476367 11.00000 0.03075 0.03645 = 0.02562 -0.00484 0.00261 0.01186 S3 6 -0.069725 0.329674 0.045905 11.00000 0.03152 0.02472 = 0.04340 0.00122 0.01337 0.00526 S4 6 0.159148 0.476313 -0.112728 11.00000 0.03157 0.02514 = 0.03633 -0.00454 0.01202 0.00265 NI1 7 -1.500000 0.000000 -0.500000 10.50000 0.02367 0.02897 = 0.02192 -0.00257 0.00263 0.00616 NI2 7 0.000000 0.500000 0.000000 10.50000 0.02307 0.02159 = 0.02917 -0.00268 0.00669 0.00193 MOLE 2 C1S 1 -0.593545 0.458394 -0.495237 10.50000 0.06863 0.09977 = 0.08273 0.00534 0.03151 0.01516 AFIX 33 H1S1 2 -0.596789 0.513875 -0.534942 10.50000 -1.50000 H1S2 2 -0.633613 0.395487 -0.540126 10.50000 -1.50000 H1S3 2 -0.478759 0.469373 -0.452432 10.50000 -1.50000 AFIX 0 C2S 1 -0.904920 0.495439 -0.458068 10.50000 0.07267 0.07862 = 0.09935 0.01039 0.02259 0.03159 AFIX 33 H2S1 2 -0.900265 0.535846 -0.512940 10.50000 -1.50000 H2S2 2 -0.865356 0.539656 -0.394762 10.50000 -1.50000 H2S3 2 -1.020131 0.452879 -0.469901 10.50000 -1.50000 AFIX 0 O1S 4 -0.698772 0.453165 -0.433714 10.50000 0.05457 0.08056 = 0.08463 0.02906 0.00776 0.01430 O2S 4 -0.800999 0.433865 -0.453090 10.50000 0.06074 0.08100 = 0.07338 0.02611 0.01663 0.01092 HKLF 4 Covalent radii and connectivity table for P-1 in P-1 C 0.770 H 0.320 N 0.700 O 0.660 P 1.100 S 1.030 NI 1.250 C1 - C6 C2 P1 C2 - C3 C1 C3 - C2 C4 C4 - O1 C5 C3 C5 - C4 C6 C6 - C1 C5 C7 - O1 C8 - O2 C9 - N1 C10 C10 - C11 C9 C11 - C10 C12 N2 C14A C12 - C11 C13 C13 - N1 C12 C14 - N2 O1S C15 C14A - N2A O2S C11 C15 - C16 C19 N2A C14 C16 - C15 C17 C17 - N3 C16 C18 - N3 C19 C19 - C18 C15 C20 - C25 C21 P2 C21 - C22 C20 C22 - C21 C23 C23 - O3 C22 C24 C24 - C23 C25 C25 - C20 C24 C26 - O3 C27 - O4 N1 - C13 C9 Ni1 N2 - C14 C11 N2A - C14A C15 N3 - C18 C17 Ni2 O1 - C4 C7 O2 - C8 P1 O3 - C23 C26 O4 - C27 P2 P1 - O2 C1 S1 S2 P2 - O4 C20 S3 S4_$4 S1 - P1 Ni1 S2 - P1 Ni1 S3 - P2 Ni2 S4 - P2_$4 Ni2 Ni1 - N1 N1_$3 S1 S1_$3 S2_$3 S2 Ni2 - N3_$4 N3 S3 S3_$4 S4_$4 S4 C1S - O1S C2S - O2S O1S - C14 C1S O2S - C2S C14A Operators for generating equivalent atoms: $1 -x-1, -y+1, -z-1 $2 -x-2, -y+1, -z-1 $3 -x-3, -y, -z-1 $4 -x, -y+1, -z 16267 Reflections read, of which 16 rejected -11 =< h =< 11, -18 =< k =< 18, -18 =< l =< 16, Max. 2-theta = 55.00 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 3 -8 2 478.33 6.48 3 35.51 0 -3 4 516.44 14.05 2 70.78 -1 0 12 42.23 1.07 3 8.11 -2 -3 13 -0.07 0.74 3 4.08 4 Inconsistent equivalents 6837 Unique reflections, of which 0 suppressed R(int) = 0.0374 R(sigma) = 0.0597 Friedel opposites merged Maximum memory for data reduction = 4152 / 69795 Special position constraints for Ni1 x = -1.5000 y = 0.0000 z = -0.5000 sof = 0.50000 Input constraints retained (at least in part) for sof Special position constraints for Ni2 x = 0.0000 y = 0.5000 z = 0.0000 sof = 0.50000 Input constraints retained (at least in part) for sof 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 = 5329 / 533027 wR2 = 0.1031 before cycle 1 for 6837 data and 412 / 412 parameters GooF = S = 1.040; Restrained GooF = 1.040 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0386 * P )^2 + 1.20 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.58269 0.00090 -0.010 OSF 2 0.00212 0.00066 0.003 EXTI Mean shift/esd = 0.008 Maximum = -0.037 for U33 S2 Max. shift = 0.000 A for H1S2 Max. dU = 0.000 for C1S Least-squares cycle 2 Maximum vector length = 511 Memory required = 5329 / 533027 wR2 = 0.1031 before cycle 2 for 6837 data and 412 / 412 parameters GooF = S = 1.040; Restrained GooF = 1.040 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0386 * P )^2 + 1.20 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.58268 0.00090 -0.015 OSF 2 0.00212 0.00066 0.003 EXTI Mean shift/esd = 0.003 Maximum = -0.015 for OSF Max. shift = 0.000 A for N2A Max. dU = 0.000 for N2A Least-squares cycle 3 Maximum vector length = 511 Memory required = 5329 / 533027 wR2 = 0.1031 before cycle 3 for 6837 data and 412 / 412 parameters GooF = S = 1.040; Restrained GooF = 1.040 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0386 * P )^2 + 1.20 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.58267 0.00090 -0.004 OSF 2 0.00212 0.00066 -0.002 EXTI Mean shift/esd = 0.000 Maximum = -0.004 for OSF Max. shift = 0.000 A for H8A Max. dU = 0.000 for N2A Least-squares cycle 4 Maximum vector length = 511 Memory required = 5329 / 533027 wR2 = 0.1031 before cycle 4 for 6837 data and 412 / 412 parameters GooF = S = 1.040; Restrained GooF = 1.040 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0386 * P )^2 + 1.20 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.58267 0.00090 0.001 OSF 2 0.00212 0.00066 -0.001 EXTI Mean shift/esd = 0.000 Maximum = 0.001 for OSF Max. shift = 0.000 A for C14 Max. dU = 0.000 for C2S Least-squares cycle 5 Maximum vector length = 511 Memory required = 5329 / 533027 wR2 = 0.1031 before cycle 5 for 6837 data and 412 / 412 parameters GooF = S = 1.040; Restrained GooF = 1.040 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0386 * P )^2 + 1.20 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.58267 0.00090 0.000 OSF 2 0.00212 0.00066 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.001 for x S2 Max. shift = 0.000 A for H7C Max. dU = 0.000 for O1S Least-squares cycle 6 Maximum vector length = 511 Memory required = 5329 / 533027 wR2 = 0.1031 before cycle 6 for 6837 data and 412 / 412 parameters GooF = S = 1.040; Restrained GooF = 1.040 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0386 * P )^2 + 1.20 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.58268 0.00090 0.001 OSF 2 0.00212 0.00066 0.001 EXTI Mean shift/esd = 0.000 Maximum = 0.001 for OSF Max. shift = 0.000 A for H8B Max. dU = 0.000 for O1S Largest correlation matrix elements 0.602 x O2S / x O1S 0.561 U12 O2S / U12 O1S 0.510 y O2S / U12 O1S 0.568 EXTI / OSF 0.544 U13 O2S / U13 O1S -0.502 U13 O2S / z O1S Idealized hydrogen atom generation before cycle 7 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2 -1.8788 0.1787 -0.8027 43 0.950 0.000 C2 C3 C1 H3 -2.1523 0.1186 -0.9069 43 0.950 0.000 C3 C2 C4 H5 -2.2684 -0.0790 -0.7184 43 0.950 0.000 C5 C4 C6 H6 -1.9927 -0.0161 -0.6107 43 0.950 0.000 C6 C1 C5 H7A -2.4693 -0.1584 -0.8719 137 0.980 0.000 C7 O1 H7A H7B -2.6148 -0.1187 -0.9353 137 0.980 0.000 C7 O1 H7A H7C -2.5373 -0.0878 -0.8167 137 0.980 0.000 C7 O1 H7A H8A -1.4100 0.2940 -0.5356 137 0.980 0.000 C8 O2 H8A H8B -1.4403 0.3631 -0.6224 137 0.980 0.000 C8 O2 H8A H8C -1.3993 0.2630 -0.6428 137 0.980 0.000 C8 O2 H8A H9 -1.2947 0.1695 -0.3293 43 0.950 0.000 C9 N1 C10 H10 -1.0475 0.2990 -0.2751 43 0.950 0.000 C10 C11 C9 H12 -0.9564 0.2309 -0.5269 43 0.950 0.000 C12 C11 C13 H13 -1.2094 0.1019 -0.5756 43 0.950 0.000 C13 N1 C12 H14 -0.6979 0.3140 -0.4171 13 1.000 0.000 C14 N2 O1S C15 H14A -0.7992 0.4179 -0.3125 13 1.000 0.000 C14A N2A O2S C11 H16 -0.4501 0.2757 -0.3008 43 0.950 0.000 C16 C15 C17 H17 -0.2057 0.3292 -0.1683 43 0.950 0.000 C17 N3 C16 H18 -0.2916 0.5758 -0.1013 43 0.950 0.000 C18 N3 C19 H19 -0.5428 0.5273 -0.2318 43 0.950 0.000 C19 C18 C15 H21 -0.3788 0.1976 0.1790 43 0.950 0.000 C21 C22 C20 H22 -0.6520 0.0931 0.1180 43 0.950 0.000 C22 C21 C23 H24 -0.7689 0.2819 -0.0790 43 0.950 0.000 C24 C23 C25 H25 -0.4928 0.3889 -0.0163 43 0.950 0.000 C25 C20 C24 H26A -1.0389 0.1830 -0.0876 137 0.980 0.000 C26 O3 H26A H26B -1.1150 0.0644 -0.1194 137 0.980 0.000 C26 O3 H26A H26C -0.9696 0.1292 -0.1585 137 0.980 0.000 C26 O3 H26A H27A 0.1007 0.3579 0.2616 137 0.980 0.000 C27 O4 H27A H27B 0.0595 0.3750 0.3624 137 0.980 0.000 C27 O4 H27A H27C 0.0899 0.4641 0.2958 137 0.980 0.000 C27 O4 H27A H1S1 -0.5968 0.5139 -0.5349 33 0.980 0.000 C1S O1S H1S1 H1S2 -0.6336 0.3955 -0.5401 33 0.980 0.000 C1S O1S H1S1 H1S3 -0.4788 0.4694 -0.4524 33 0.980 0.000 C1S O1S H1S1 H2S1 -0.9003 0.5359 -0.5129 33 0.980 0.000 C2S O2S H2S1 H2S2 -0.8654 0.5397 -0.3948 33 0.980 0.000 C2S O2S H2S1 H2S3 -1.0201 0.4529 -0.4699 33 0.980 0.000 C2S O2S H2S1 P-1 in P-1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 -1.90729 0.08704 -0.69579 1.00000 0.02983 0.03224 0.02588 0.00117 0.00504 0.01290 0.02963 0.00649 0.00037 0.00022 0.00022 0.00000 0.00160 0.00158 0.00162 0.00125 0.00129 0.00137 0.00068 C2 -1.95752 0.12655 -0.78493 1.00000 0.03792 0.03672 0.03631 0.00993 0.00652 0.01055 0.03849 0.00722 0.00042 0.00024 0.00024 0.00000 0.00185 0.00175 0.00189 0.00143 0.00151 0.00150 0.00078 H2 -1.87882 0.17870 -0.80269 1.00000 0.04618 0.00000 0.00000 C3 -2.11939 0.09065 -0.84687 1.00000 0.04142 0.04576 0.03568 0.01114 0.00256 0.01609 0.04266 0.00754 0.00043 0.00025 0.00025 0.00000 0.00198 0.00198 0.00194 0.00154 0.00157 0.00168 0.00085 H3 -2.15227 0.11863 -0.90692 1.00000 0.05119 0.00000 0.00000 C4 -2.23574 0.01389 -0.82282 1.00000 0.03038 0.03757 0.02734 -0.00391 0.00017 0.01412 0.03334 0.00658 0.00038 0.00023 0.00022 0.00000 0.00167 0.00173 0.00170 0.00134 0.00134 0.00145 0.00073 C5 -2.18916 -0.02639 -0.73516 1.00000 0.03318 0.04466 0.02931 0.00294 0.01120 0.01272 0.03546 0.00714 0.00040 0.00025 0.00023 0.00000 0.00172 0.00185 0.00174 0.00140 0.00139 0.00150 0.00074 H5 -2.26837 -0.07905 -0.71836 1.00000 0.04255 0.00000 0.00000 C6 -2.02475 0.01092 -0.67150 1.00000 0.03375 0.04318 0.02596 0.00529 0.00471 0.01557 0.03469 0.00690 0.00039 0.00024 0.00023 0.00000 0.00174 0.00182 0.00167 0.00136 0.00137 0.00151 0.00074 H6 -1.99271 -0.01608 -0.61072 1.00000 0.04163 0.00000 0.00000 C7 -2.51263 -0.10194 -0.87774 1.00000 0.03077 0.05391 0.04379 -0.00999 0.00789 0.00955 0.04512 0.00729 0.00041 0.00027 0.00026 0.00000 0.00182 0.00217 0.00207 0.00169 0.00156 0.00168 0.00088 H7A -2.46932 -0.15844 -0.87189 1.00000 0.06768 0.00000 0.00000 H7B -2.61481 -0.11868 -0.93534 1.00000 0.06768 0.00000 0.00000 H7C -2.53730 -0.08785 -0.81666 1.00000 0.06768 0.00000 0.00000 C8 -1.45633 0.29410 -0.60788 1.00000 0.04898 0.04261 0.07457 0.00831 0.00269 -0.00322 0.06358 0.00834 0.00048 0.00028 0.00033 0.00000 0.00241 0.00217 0.00295 0.00200 0.00212 0.00187 0.00120 H8A -1.41003 0.29401 -0.53563 1.00000 0.09537 0.00000 0.00000 H8B -1.44030 0.36315 -0.62238 1.00000 0.09537 0.00000 0.00000 H8C -1.39929 0.26304 -0.64276 1.00000 0.09537 0.00000 0.00000 C9 -1.22491 0.18161 -0.37013 1.00000 0.03682 0.04133 0.03738 -0.00820 0.00334 0.00782 0.04194 0.00697 0.00042 0.00025 0.00025 0.00000 0.00187 0.00187 0.00190 0.00152 0.00151 0.00157 0.00083 H9 -1.29467 0.16946 -0.32927 1.00000 0.05033 0.00000 0.00000 C10 -1.07772 0.25922 -0.33742 1.00000 0.04258 0.05022 0.05267 -0.01322 -0.00305 0.00289 0.05605 0.00788 0.00048 0.00028 0.00030 0.00000 0.00221 0.00227 0.00237 0.00185 0.00188 0.00185 0.00106 H10 -1.04747 0.29905 -0.27507 1.00000 0.06726 0.00000 0.00000 C11 -0.97421 0.27950 -0.39430 1.00000 0.02759 0.05338 0.08408 -0.01463 -0.00111 0.00115 0.06279 0.00823 0.00046 0.00030 0.00036 0.00000 0.00194 0.00239 0.00315 0.00224 0.00204 0.00176 0.00120 C12 -1.02431 0.21945 -0.48494 1.00000 0.03340 0.04820 0.08422 0.01168 0.02603 0.01027 0.05424 0.00884 0.00045 0.00028 0.00033 0.00000 0.00194 0.00218 0.00301 0.00209 0.00200 0.00173 0.00102 H12 -0.95645 0.23090 -0.52694 1.00000 0.06508 0.00000 0.00000 C13 -1.17550 0.14226 -0.51315 1.00000 0.03067 0.04027 0.04600 0.00414 0.01082 0.01121 0.03943 0.00752 0.00040 0.00025 0.00026 0.00000 0.00174 0.00183 0.00204 0.00153 0.00155 0.00151 0.00079 H13 -1.20938 0.10194 -0.57565 1.00000 0.04732 0.00000 0.00000 C14 -0.68590 0.37451 -0.37315 0.50000 0.04936 0.01830 0.00103 0.00065 0.00060 0.00000 0.00201 H14 -0.69793 0.31403 -0.41709 0.50000 0.05923 0.00000 0.00000 C14A -0.81218 0.37409 -0.37326 0.50000 0.04840 0.01816 0.00103 0.00059 0.00066 0.00000 0.00199 H14A -0.79920 0.41793 -0.31248 0.50000 0.05808 0.00000 0.00000 C15 -0.52602 0.39406 -0.27955 1.00000 0.02862 0.08642 0.05021 -0.01692 0.00262 -0.00077 0.06253 0.00820 0.00046 0.00035 0.00030 0.00000 0.00195 0.00313 0.00240 0.00224 0.00172 0.00206 0.00119 C16 -0.42139 0.33732 -0.26008 1.00000 0.03948 0.05521 0.05019 -0.01486 0.00280 -0.00345 0.05587 0.00779 0.00047 0.00030 0.00028 0.00000 0.00212 0.00233 0.00236 0.00187 0.00178 0.00187 0.00105 H16 -0.45011 0.27569 -0.30075 1.00000 0.06704 0.00000 0.00000 C17 -0.27493 0.37036 -0.18137 1.00000 0.03603 0.03651 0.04269 -0.00813 0.00823 0.00081 0.04229 0.00697 0.00042 0.00025 0.00025 0.00000 0.00185 0.00179 0.00198 0.00152 0.00154 0.00151 0.00083 H17 -0.20570 0.32921 -0.16830 1.00000 0.05075 0.00000 0.00000 C18 -0.32472 0.51360 -0.14202 1.00000 0.03104 0.04381 0.04119 0.00450 0.01366 0.00874 0.03902 0.00749 0.00040 0.00026 0.00025 0.00000 0.00174 0.00190 0.00194 0.00152 0.00150 0.00153 0.00078 H18 -0.29161 0.57579 -0.10133 1.00000 0.04682 0.00000 0.00000 C19 -0.47530 0.48507 -0.21969 1.00000 0.03304 0.08494 0.04954 0.01136 0.01267 0.02449 0.05466 0.00890 0.00045 0.00033 0.00028 0.00000 0.00196 0.00298 0.00230 0.00212 0.00172 0.00203 0.00102 H19 -0.54281 0.52726 -0.23175 1.00000 0.06560 0.00000 0.00000 C20 -0.40706 0.30451 0.08690 1.00000 0.03208 0.02765 0.03084 -0.00006 0.01347 0.00438 0.03073 0.00654 0.00038 0.00021 0.00022 0.00000 0.00166 0.00152 0.00168 0.00126 0.00137 0.00133 0.00069 C21 -0.45731 0.21526 0.12669 1.00000 0.03880 0.03789 0.03725 0.01010 0.01330 0.00658 0.03898 0.00739 0.00042 0.00024 0.00025 0.00000 0.00187 0.00179 0.00188 0.00146 0.00150 0.00153 0.00078 H21 -0.37885 0.19757 0.17904 1.00000 0.04677 0.00000 0.00000 C22 -0.61941 0.15337 0.09031 1.00000 0.04125 0.03539 0.04302 0.01393 0.01586 0.00189 0.04160 0.00743 0.00042 0.00024 0.00025 0.00000 0.00196 0.00178 0.00204 0.00151 0.00164 0.00156 0.00083 H22 -0.65205 0.09312 0.11802 1.00000 0.04992 0.00000 0.00000 C23 -0.73616 0.17707 0.01407 1.00000 0.02894 0.03103 0.03881 -0.00260 0.01600 -0.00005 0.03417 0.00670 0.00038 0.00023 0.00024 0.00000 0.00165 0.00161 0.00185 0.00137 0.00144 0.00136 0.00073 C24 -0.68970 0.26496 -0.02649 1.00000 0.03217 0.03165 0.04155 0.00166 0.01177 0.00881 0.03557 0.00705 0.00040 0.00023 0.00025 0.00000 0.00171 0.00164 0.00189 0.00139 0.00146 0.00141 0.00074 H24 -0.76890 0.28191 -0.07904 1.00000 0.04269 0.00000 0.00000 C25 -0.52490 0.32826 0.01092 1.00000 0.03586 0.02730 0.04438 0.00584 0.01808 0.00659 0.03546 0.00702 0.00039 0.00023 0.00024 0.00000 0.00179 0.00156 0.00194 0.00137 0.00153 0.00140 0.00074 H25 -0.49282 0.38891 -0.01628 1.00000 0.04256 0.00000 0.00000 C26 -1.01327 0.12240 -0.10214 1.00000 0.02960 0.04344 0.05232 -0.01141 0.01042 0.00586 0.04422 0.00714 0.00040 0.00026 0.00026 0.00000 0.00177 0.00195 0.00218 0.00165 0.00162 0.00155 0.00086 H26A -1.03889 0.18299 -0.08759 1.00000 0.06633 0.00000 0.00000 H26B -1.11496 0.06441 -0.11938 1.00000 0.06633 0.00000 0.00000 H26C -0.96957 0.12920 -0.15850 1.00000 0.06633 0.00000 0.00000 C27 0.04360 0.39154 0.29395 1.00000 0.04647 0.07193 0.04339 0.00854 -0.00628 0.00027 0.06314 0.00821 0.00047 0.00032 0.00029 0.00000 0.00235 0.00278 0.00230 0.00198 0.00183 0.00208 0.00120 H27A 0.10067 0.35791 0.26160 1.00000 0.09471 0.00000 0.00000 H27B 0.05952 0.37504 0.36237 1.00000 0.09471 0.00000 0.00000 H27C 0.08994 0.46409 0.29579 1.00000 0.09471 0.00000 0.00000 N1 -1.27562 0.12173 -0.45726 1.00000 0.02697 0.03266 0.03019 -0.00207 0.00389 0.00863 0.03155 0.00529 0.00030 0.00018 0.00018 0.00000 0.00134 0.00135 0.00142 0.00110 0.00113 0.00113 0.00059 N2 -0.81765 0.35069 -0.33266 0.50000 0.06140 0.01673 0.00093 0.00055 0.00061 0.00000 0.00202 H2N -0.80615 0.37845 -0.27320 0.50000 0.07368 0.00000 0.00000 N2A -0.68313 0.33258 -0.35162 0.50000 0.05929 0.01632 0.00090 0.00059 0.00054 0.00000 0.00193 H2AN -0.69602 0.27318 -0.38019 0.50000 0.07114 0.00000 0.00000 N3 -0.22399 0.45748 -0.12183 1.00000 0.02482 0.03017 0.03376 -0.00155 0.00783 0.00268 0.03154 0.00527 0.00030 0.00018 0.00018 0.00000 0.00130 0.00133 0.00144 0.00110 0.00110 0.00111 0.00059 O1 -2.39199 -0.01651 -0.89121 1.00000 0.03086 0.05088 0.04005 0.00130 -0.00325 0.01283 0.04421 0.00486 0.00027 0.00017 0.00017 0.00000 0.00124 0.00142 0.00135 0.00109 0.00104 0.00111 0.00059 O2 -1.63302 0.23800 -0.64174 1.00000 0.04411 0.03210 0.04585 0.00349 0.00253 0.00536 0.04514 0.00488 0.00029 0.00016 0.00017 0.00000 0.00140 0.00120 0.00140 0.00103 0.00112 0.00107 0.00060 O3 -0.89241 0.10880 -0.01683 1.00000 0.03269 0.03962 0.04912 0.00218 0.01318 -0.00261 0.04389 0.00490 0.00028 0.00017 0.00017 0.00000 0.00126 0.00128 0.00143 0.00108 0.00109 0.00105 0.00058 O4 -0.13262 0.35845 0.23796 1.00000 0.04290 0.04798 0.03208 0.00700 0.00706 0.00477 0.04443 0.00496 0.00029 0.00017 0.00016 0.00000 0.00138 0.00137 0.00127 0.00104 0.00105 0.00113 0.00059 P1 -1.69159 0.12404 -0.62132 1.00000 0.02998 0.03162 0.02781 0.00082 0.00380 0.00919 0.03134 0.00174 0.00010 0.00006 0.00006 0.00000 0.00042 0.00042 0.00043 0.00033 0.00034 0.00035 0.00020 P2 -0.19165 0.37882 0.12396 1.00000 0.02978 0.02803 0.03204 0.00116 0.00944 0.00301 0.03161 0.00175 0.00010 0.00006 0.00006 0.00000 0.00042 0.00040 0.00045 0.00033 0.00035 0.00034 0.00020 S1 -1.56956 0.04593 -0.67036 1.00000 0.03153 0.04388 0.02462 0.00145 0.00592 0.01281 0.03399 0.00172 0.00010 0.00006 0.00006 0.00000 0.00042 0.00046 0.00041 0.00033 0.00032 0.00036 0.00020 S2 -1.65915 0.11274 -0.47637 1.00000 0.03074 0.03644 0.02560 -0.00484 0.00260 0.01185 0.03241 0.00165 0.00010 0.00006 0.00006 0.00000 0.00041 0.00042 0.00040 0.00031 0.00032 0.00034 0.00019 S3 -0.06973 0.32967 0.04591 1.00000 0.03152 0.02471 0.04339 0.00121 0.01336 0.00526 0.03387 0.00172 0.00010 0.00005 0.00006 0.00000 0.00042 0.00038 0.00048 0.00033 0.00036 0.00033 0.00020 S4 0.15915 0.47631 -0.11273 1.00000 0.03156 0.02514 0.03631 -0.00454 0.01201 0.00264 0.03247 0.00166 0.00010 0.00005 0.00006 0.00000 0.00041 0.00037 0.00044 0.00031 0.00034 0.00032 0.00019 Ni1 -1.50000 0.00000 -0.50000 0.50000 0.02366 0.02896 0.02191 -0.00258 0.00262 0.00616 0.02662 0.00000 0.00000 0.00000 0.00000 0.00000 0.00028 0.00028 0.00028 0.00021 0.00022 0.00023 0.00015 Ni2 0.00000 0.50000 0.00000 0.50000 0.02306 0.02158 0.02916 -0.00268 0.00669 0.00193 0.02637 0.00000 0.00000 0.00000 0.00000 0.00000 0.00028 0.00026 0.00030 0.00021 0.00022 0.00022 0.00015 C1S -0.59355 0.45841 -0.49525 0.50000 0.06866 0.09990 0.08285 0.00533 0.03160 0.01525 0.08508 0.02344 0.00125 0.00082 0.00079 0.00000 0.00654 0.00799 0.00704 0.00592 0.00590 0.00582 0.00303 H1S1 -0.59681 0.51389 -0.53495 0.50000 0.12761 0.00000 0.00000 H1S2 -0.63360 0.39550 -0.54014 0.50000 0.12761 0.00000 0.00000 H1S3 -0.47876 0.46939 -0.45244 0.50000 0.12761 0.00000 0.00000 C2S -0.90493 0.49545 -0.45807 0.50000 0.07265 0.07875 0.09948 0.01037 0.02265 0.03165 0.08317 0.02345 0.00125 0.00077 0.00081 0.00000 0.00668 0.00656 0.00814 0.00578 0.00585 0.00583 0.00299 H2S1 -0.90027 0.53585 -0.51295 0.50000 0.12475 0.00000 0.00000 H2S2 -0.86538 0.53967 -0.39477 0.50000 0.12475 0.00000 0.00000 H2S3 -1.02014 0.45288 -0.46991 0.50000 0.12475 0.00000 0.00000 O1S -0.69879 0.45315 -0.43372 0.50000 0.05461 0.08072 0.08461 0.02913 0.00774 0.01438 0.07806 0.01798 0.00099 0.00061 0.00062 0.00000 0.00430 0.00516 0.00538 0.00393 0.00463 0.00446 0.00237 O2S -0.80099 0.43387 -0.45308 0.50000 0.06076 0.08101 0.07348 0.02614 0.01665 0.01092 0.07534 0.01793 0.00101 0.00060 0.00058 0.00000 0.00449 0.00506 0.00507 0.00377 0.00438 0.00472 0.00221 Final Structure Factor Calculation for P-1 in P-1 Total number of l.s. parameters = 412 Maximum vector length = 511 Memory required = 4917 / 26061 wR2 = 0.1031 before cycle 7 for 6837 data and 0 / 412 parameters GooF = S = 1.040; Restrained GooF = 1.040 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0386 * P )^2 + 1.20 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0419 for 4807 Fo > 4sig(Fo) and 0.0756 for all 6837 data wR2 = 0.1031, GooF = S = 1.040, Restrained GooF = 1.040 for all data Occupancy sum of asymmetric unit = 43.00 for non-hydrogen and 33.00 for hydrogen atoms Principal mean square atomic displacements U 0.0370 0.0275 0.0243 C1 0.0498 0.0362 0.0295 C2 0.0558 0.0460 0.0262 C3 0.0483 0.0300 0.0218 C4 0.0454 0.0330 0.0280 C5 0.0438 0.0367 0.0236 C6 0.0686 0.0367 0.0301 C7 0.0994 0.0594 0.0319 C8 0.0554 0.0445 0.0259 C9 0.0776 0.0645 0.0260 C10 0.1048 0.0603 0.0232 C11 0.0843 0.0502 0.0282 C12 0.0474 0.0405 0.0304 C13 0.1086 0.0548 0.0242 C15 0.0808 0.0619 0.0249 C16 0.0568 0.0453 0.0248 C17 0.0466 0.0410 0.0295 C18 0.0851 0.0500 0.0288 C19 0.0403 0.0265 0.0254 C20 0.0493 0.0387 0.0290 C21 0.0581 0.0440 0.0227 C22 0.0504 0.0303 0.0218 C23 0.0430 0.0330 0.0307 C24 0.0461 0.0350 0.0254 C25 0.0689 0.0354 0.0284 C26 0.1019 0.0585 0.0290 C27 0.0398 0.0311 0.0238 N1 0.0397 0.0328 0.0221 N3 0.0582 0.0511 0.0233 O1 0.0655 0.0398 0.0301 O2 0.0577 0.0494 0.0245 O3 0.0635 0.0386 0.0311 O4 0.0373 0.0323 0.0245 P1 0.0383 0.0324 0.0240 P2 0.0449 0.0330 0.0241 S1 0.0448 0.0311 0.0213 S2 0.0446 0.0331 0.0239 S3 0.0445 0.0316 0.0212 S4 0.0333 0.0286 0.0180 Ni1 0.0336 0.0280 0.0175 Ni2 0.1118 0.0815 0.0619 C1S 0.1035 0.0816 0.0644 C2S 0.1199 0.0630 0.0513 O1S 0.1089 0.0617 0.0553 O2S Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.013 0.027 0.040 0.055 0.073 0.091 0.116 0.152 0.218 1.000 Number in group 689. 733. 629. 709. 683. 662. 677. 693. 675. 687. GooF 0.892 0.923 0.981 1.055 1.081 1.162 1.109 1.059 1.134 0.979 K 1.439 0.944 0.900 0.925 0.943 0.956 0.981 1.000 1.022 1.010 Resolution(A) 0.77 0.80 0.84 0.88 0.93 0.99 1.07 1.17 1.34 1.68 inf Number in group 705. 665. 694. 676. 686. 684. 685. 675. 683. 684. GooF 1.002 0.992 1.032 0.984 1.041 1.045 1.088 0.911 0.856 1.366 K 0.968 0.990 0.999 0.996 1.010 1.024 1.025 1.017 1.007 0.996 R1 0.235 0.183 0.163 0.101 0.091 0.067 0.052 0.038 0.026 0.028 Recommended weighting scheme: WGHT 0.0384 1.2054 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 3 0 175.70 96.72 5.44 0.056 4.57 0 4 4 604.45 428.17 5.26 0.117 2.22 4 -9 11 0.97 22.48 4.83 0.027 0.88 -4 5 14 44.51 256.22 4.65 0.091 0.94 -6 -2 12 255.75 427.92 4.57 0.117 1.00 -1 -8 12 219.83 348.19 4.46 0.106 0.99 -5 11 6 227.46 352.16 4.45 0.106 1.08 0 1 2 662.77 866.93 4.38 0.167 5.69 0 4 3 162.51 247.61 4.37 0.089 2.52 -6 -2 10 -19.32 181.13 4.24 0.076 1.10 0 2 1 653.93 847.11 4.20 0.165 5.69 -1 0 3 181.88 90.69 4.19 0.054 4.57 0 3 2 791.59 999.41 4.05 0.179 3.50 -1 -5 2 682.05 882.51 4.04 0.168 2.35 0 2 3 787.41 993.17 4.01 0.178 3.50 -2 7 13 40.60 108.44 3.98 0.059 0.92 1 14 7 66.10 198.60 3.94 0.080 0.78 4 -10 5 132.77 241.49 3.90 0.088 1.15 -1 0 12 124.42 240.11 3.88 0.088 1.16 3 1 0 1543.11 1266.56 3.83 0.201 2.47 -2 -7 13 182.97 287.10 3.83 0.096 0.96 5 5 3 87.96 34.06 3.75 0.033 1.09 1 -2 5 686.18 853.22 3.70 0.165 2.35 3 0 1 1538.35 1274.98 3.68 0.202 2.47 -4 1 1 1725.42 2085.46 3.61 0.259 2.17 6 2 2 398.17 290.71 3.55 0.097 1.15 -4 6 1 620.09 774.11 3.54 0.157 1.84 2 -3 6 33.91 11.11 3.53 0.019 1.76 0 4 5 9.19 35.41 3.47 0.034 1.96 1 -1 2 959.96 1163.74 3.45 0.193 4.63 0 5 4 11.77 39.67 3.45 0.036 1.97 0 2 13 21.07 64.65 3.41 0.046 1.00 6 -4 10 75.91 222.58 3.40 0.084 0.86 -11 7 3 29.16 204.56 3.39 0.081 0.80 0 -11 10 -6.32 61.77 3.38 0.044 0.96 -1 9 13 125.17 279.39 3.37 0.095 0.83 0 7 13 991.99 721.32 3.35 0.152 0.86 -6 9 8 369.49 270.80 3.30 0.093 1.08 8 3 2 -8.59 59.50 3.28 0.044 0.87 8 4 4 21.88 114.35 3.25 0.061 0.79 1 7 14 20.77 190.54 3.22 0.078 0.78 -9 -6 9 -58.34 70.60 3.21 0.048 0.77 8 1 4 183.59 291.34 3.20 0.097 0.87 5 0 5 172.02 243.77 3.19 0.088 1.21 -4 1 6 639.44 788.29 3.19 0.159 1.84 -6 6 16 1125.71 828.20 3.18 0.163 0.81 2 4 3 311.26 234.96 3.17 0.087 1.81 -5 12 11 92.15 320.59 3.16 0.101 0.85 2 -5 4 487.70 392.76 3.12 0.112 2.00 1 8 10 446.26 595.16 3.12 0.138 0.93 Bond lengths and angles C1 - Distance Angles C6 1.3886 (0.0044) C2 1.3972 (0.0043) 118.64 (0.28) P1 1.7927 (0.0030) 120.42 (0.23) 120.58 (0.25) C1 - C6 C2 C2 - Distance Angles C3 1.3693 (0.0046) C1 1.3972 (0.0043) 120.47 (0.32) C2 - C3 C3 - Distance Angles C2 1.3693 (0.0045) C4 1.3862 (0.0048) 120.66 (0.31) C3 - C2 C4 - Distance Angles O1 1.3642 (0.0035) C5 1.3806 (0.0044) 124.87 (0.30) C3 1.3862 (0.0048) 115.17 (0.28) 119.96 (0.29) C4 - O1 C5 C5 - Distance Angles C4 1.3806 (0.0044) C6 1.3947 (0.0043) 119.40 (0.31) C5 - C4 C6 - Distance Angles C1 1.3886 (0.0044) C5 1.3947 (0.0043) 120.86 (0.29) C6 - C1 C7 - Distance Angles O1 1.4156 (0.0042) C7 - C8 - Distance Angles O2 1.4507 (0.0043) C8 - C9 - Distance Angles N1 1.3457 (0.0039) C10 1.3697 (0.0049) 123.28 (0.37) C9 - N1 C10 - Distance Angles C11 1.3677 (0.0061) C9 1.3697 (0.0049) 120.16 (0.36) C10 - C11 C11 - Distance Angles C10 1.3677 (0.0061) C12 1.3874 (0.0058) 117.73 (0.35) N2 1.4459 (0.0079) 107.14 (0.48) 133.92 (0.51) C14A 1.5862 (0.0089) 125.85 (0.47) 115.94 (0.50) 25.29 (0.37) C11 - C10 C12 N2 C12 - Distance Angles C11 1.3874 (0.0058) C13 1.3891 (0.0047) 118.79 (0.39) C12 - C11 C13 - Distance Angles N1 1.3332 (0.0042) C12 1.3891 (0.0047) 123.53 (0.34) C13 - N1 C14 - Distance Angles N2 1.4091 (0.0115) O1S 1.4335 (0.0111) 109.07 (0.77) C15 1.5692 (0.0087) 103.88 (0.63) 118.64 (0.65) C14 - N2 O1S C14A - Distance Angles N2A 1.3979 (0.0111) O2S 1.4385 (0.0112) 108.83 (0.80) C11 1.5862 (0.0089) 103.31 (0.61) 117.34 (0.65) C14A - N2A O2S C15 - Distance Angles C16 1.3737 (0.0059) C19 1.3896 (0.0057) 117.80 (0.33) N2A 1.4529 (0.0077) 107.30 (0.45) 133.96 (0.48) C14 1.5692 (0.0087) 126.13 (0.46) 115.38 (0.48) 25.55 (0.36) C15 - C16 C19 N2A C16 - Distance Angles C15 1.3737 (0.0059) C17 1.3740 (0.0047) 119.51 (0.36) C16 - C15 C17 - Distance Angles N3 1.3429 (0.0039) C16 1.3740 (0.0047) 123.78 (0.35) C17 - N3 C18 - Distance Angles N3 1.3399 (0.0041) C19 1.3889 (0.0047) 123.04 (0.33) C18 - N3 C19 - Distance Angles C18 1.3889 (0.0047) C15 1.3896 (0.0058) 119.20 (0.38) C19 - C18 C20 - Distance Angles C25 1.3858 (0.0043) C21 1.4005 (0.0043) 118.40 (0.29) P2 1.7899 (0.0031) 120.77 (0.23) 120.49 (0.25) C20 - C25 C21 C21 - Distance Angles C22 1.3709 (0.0046) C20 1.4005 (0.0043) 120.19 (0.31) C21 - C22 C22 - Distance Angles C21 1.3709 (0.0046) C23 1.3818 (0.0046) 121.18 (0.30) C22 - C21 C23 - Distance Angles O3 1.3634 (0.0036) C22 1.3818 (0.0046) 115.71 (0.28) C24 1.3853 (0.0044) 124.52 (0.29) 119.77 (0.29) C23 - O3 C22 C24 - Distance Angles C23 1.3853 (0.0044) C25 1.3958 (0.0043) 119.06 (0.30) C24 - C23 C25 - Distance Angles C20 1.3858 (0.0043) C24 1.3958 (0.0043) 121.40 (0.29) C25 - C20 C26 - Distance Angles O3 1.4163 (0.0040) C26 - C27 - Distance Angles O4 1.4471 (0.0042) C27 - N1 - Distance Angles C13 1.3332 (0.0042) C9 1.3457 (0.0039) 116.51 (0.29) Ni1 2.1126 (0.0024) 122.42 (0.21) 121.06 (0.23) N1 - C13 C9 N2 - Distance Angles C14 1.4091 (0.0115) C11 1.4459 (0.0079) 116.77 (0.68) N2 - C14 N2A - Distance Angles C14A 1.3979 (0.0111) C15 1.4529 (0.0077) 115.75 (0.65) N2A - C14A N3 - Distance Angles C18 1.3399 (0.0041) C17 1.3429 (0.0039) 116.63 (0.28) Ni2 2.1113 (0.0024) 122.30 (0.21) 121.03 (0.23) N3 - C18 C17 O1 - Distance Angles C4 1.3642 (0.0035) C7 1.4156 (0.0042) 118.45 (0.26) O1 - C4 O2 - Distance Angles C8 1.4507 (0.0043) P1 1.6011 (0.0023) 118.85 (0.22) O2 - C8 O3 - Distance Angles C23 1.3634 (0.0036) C26 1.4163 (0.0040) 118.73 (0.26) O3 - C23 O4 - Distance Angles C27 1.4471 (0.0042) P2 1.6015 (0.0023) 119.14 (0.23) O4 - C27 P1 - Distance Angles O2 1.6011 (0.0023) C1 1.7927 (0.0030) 99.76 (0.13) S1 1.9970 (0.0011) 110.84 (0.11) 111.89 (0.10) S2 1.9989 (0.0011) 112.16 (0.10) 112.64 (0.11) 109.32 (0.05) P1 - O2 C1 S1 P2 - Distance Angles O4 1.6015 (0.0023) C20 1.7899 (0.0031) 99.94 (0.13) S3 1.9963 (0.0012) 110.69 (0.10) 111.84 (0.10) S4_$4 1.9979 (0.0011) 112.12 (0.10) 112.62 (0.11) 109.38 (0.05) P2 - O4 C20 S3 S1 - Distance Angles P1 1.9970 (0.0011) Ni1 2.4577 (0.0008) 84.72 (0.04) S1 - P1 S2 - Distance Angles P1 1.9989 (0.0011) Ni1 2.4980 (0.0008) 83.62 (0.04) S2 - P1 S3 - Distance Angles P2 1.9963 (0.0012) Ni2 2.4574 (0.0008) 84.69 (0.03) S3 - P2 S4 - Distance Angles P2_$4 1.9979 (0.0011) Ni2 2.4978 (0.0008) 83.59 (0.04) S4 - P2_$4 Ni1 - Distance Angles N1 2.1126 (0.0024) N1_$3 2.1126 (0.0024) 180.00 (0.19) S1 2.4577 (0.0008) 89.77 (0.07) 90.23 (0.07) S1_$3 2.4577 (0.0008) 90.23 (0.07) 89.77 (0.07) 180.00 (0.02) S2_$3 2.4980 (0.0008) 89.04 (0.07) 90.96 (0.07) 97.74 (0.03) 82.26 (0.03) S2 2.4980 (0.0008) 90.96 (0.07) 89.04 (0.07) 82.26 (0.03) 97.74 (0.03) 180.00 (0.03) Ni1 - N1 N1_$3 S1 S1_$3 S2_$3 Ni2 - Distance Angles N3_$4 2.1113 (0.0024) N3 2.1113 (0.0024) 180.00 S3 2.4574 (0.0008) 89.70 (0.07) 90.30 (0.07) S3_$4 2.4574 (0.0008) 90.30 (0.07) 89.70 (0.07) 180.00 (0.01) S4_$4 2.4978 (0.0008) 90.89 (0.07) 89.11 (0.07) 82.26 (0.03) 97.74 (0.03) S4 2.4978 (0.0008) 89.11 (0.07) 90.89 (0.07) 97.74 (0.03) 82.26 (0.03) 180.00 Ni2 - N3_$4 N3 S3 S3_$4 S4_$4 C1S - Distance Angles O1S 1.4429 (0.0128) C1S - C2S - Distance Angles O2S 1.4347 (0.0121) C2S - O1S - Distance Angles C14 1.4335 (0.0112) C1S 1.4429 (0.0128) 108.37 (0.80) O1S - C14 O2S - Distance Angles C2S 1.4347 (0.0121) C14A 1.4385 (0.0112) 108.43 (0.81) O2S - C2S FMAP and GRID set by program FMAP 2 2 35 GRID -1.563 -2 -2 1.563 2 2 R1 = 0.0739 for 6837 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.64 at 0.2065 0.3137 0.5984 [ 0.94 A from H14 ] Deepest hole -0.43 at 0.3747 0.3712 0.6701 [ 0.62 A from N2A ] Mean = 0.00, Rms deviation from mean = 0.08 e/A^3, Highest memory used = 4597 / 29895 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 -0.7935 0.3137 -0.4016 1.00000 0.05 0.64 0.94 H14 0.97 N2A 1.01 C14A 1.04 C14 Q2 1 -0.7121 0.4062 -0.3055 1.00000 0.05 0.59 0.82 H14A 0.98 N2 1.05 H2N 1.07 C14A Q3 1 -0.5562 0.4247 -0.2399 1.00000 0.05 0.48 0.85 C15 0.91 C19 1.42 H19 1.84 N2A Q4 1 -0.9501 0.2299 -0.4266 1.00000 0.05 0.38 0.86 C12 0.93 C11 1.40 H12 1.95 N2 Q5 1 -1.3070 0.1213 -0.6194 1.00000 0.05 0.36 1.02 H13 1.56 C13 2.13 S1 2.22 N1 Shortest distances between peaks (including symmetry equivalents) 2 3 1.36 1 4 1.47 1 2 1.68 1 3 2.65 2 4 2.83 Time profile in seconds ----------------------- 0.06: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.01: 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. 0.88: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.01: OSF, H-atoms from difference map 0.02: Set up l.s. refinement 0.00: Generate idealized H-atoms 4.06: Structure factors and derivatives 14.79: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 1.01: Solve l.s. equations 0.00: Generate HTAB table 0.04: Other dependent quantities, CIF, tables 0.28: Analysis of variance 0.07: Merge reflections for Fourier and .fcf 0.07: Fourier summations 0.05: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + p-1 finished at 15:57:32 Total CPU time: 21.6 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++