+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2006slh0985 started at 12:16:58 on 16-Nov-2006 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2006slh0985 in P-1 CELL 0.71073 9.1961 10.5439 12.5033 113.948 98.202 95.732 ZERR 2.00 0.0003 0.0004 0.0004 0.002 0.002 0.002 LATT 1 SFAC C H N O P S FE NI UNIT 42 44 2 4 2 4 1 1 V = 1079.84 F(000) = 490.0 Mu = 1.08 mm-1 Cell Wt = 945.53 Rho = 1.454 MERG 2 OMIT -3.00 55.00 OMIT 0 0 1 OMIT 1 0 0 OMIT -1 -1 1 EXTI 0.00478 FMAP 2 PLAN 5 SIZE 0.06 0.08 0.24 ACTA WGHT 0.03370 0.92500 L.S. 6 TEMP -153.00 FVAR 0.71746 MOLE 1 C1 1 -0.263455 0.169410 0.279335 11.00000 0.02650 0.02999 = 0.02555 0.01101 0.00360 0.00717 C2 1 -0.369390 0.047393 0.232576 11.00000 0.03080 0.03626 = 0.04277 0.01989 -0.00613 0.00628 AFIX 43 H2 2 -0.347001 -0.030972 0.247041 11.00000 -1.20000 AFIX 0 C3 1 -0.508048 0.037059 0.164801 11.00000 0.02942 0.03425 = 0.04396 0.01901 -0.00457 -0.00023 AFIX 43 H3 2 -0.579377 -0.047345 0.133283 11.00000 -1.20000 AFIX 0 C4 1 -0.540275 0.151908 0.144089 11.00000 0.02447 0.03816 = 0.03277 0.01713 -0.00007 0.00518 C5 1 -0.435655 0.275475 0.191457 11.00000 0.03126 0.03366 = 0.04332 0.01928 -0.00019 0.00371 AFIX 43 H5 2 -0.458325 0.354149 0.177600 11.00000 -1.20000 AFIX 0 C6 1 -0.298670 0.284169 0.258695 11.00000 0.02900 0.03261 = 0.03395 0.01264 0.00126 0.00172 AFIX 43 H6 2 -0.227986 0.369089 0.291082 11.00000 -1.20000 AFIX 0 C7 1 -0.787227 0.034832 0.033131 11.00000 0.02301 0.04832 = 0.05049 0.02477 -0.00702 -0.00340 AFIX 137 H7A 2 -0.749350 -0.050148 -0.013515 11.00000 -1.50000 H7B 2 -0.870423 0.047555 -0.017848 11.00000 -1.50000 H7C 2 -0.821832 0.024976 0.100408 11.00000 -1.50000 AFIX 0 C8 1 0.149948 0.382338 0.440836 11.00000 0.02621 0.04494 = 0.04079 0.01056 -0.00037 -0.00096 AFIX 23 H8A 2 0.167090 0.354164 0.507473 11.00000 -1.20000 H8B 2 0.157861 0.486094 0.475588 11.00000 -1.20000 AFIX 0 C9 1 0.266358 0.340571 0.367996 11.00000 0.04072 0.07581 = 0.05999 0.03391 0.01109 0.00867 AFIX 137 H9A 2 0.267473 0.239687 0.342269 11.00000 -1.50000 H9B 2 0.364184 0.394538 0.416103 11.00000 -1.50000 H9C 2 0.244049 0.359993 0.297666 11.00000 -1.50000 AFIX 0 O1 4 0.000885 0.316706 0.369227 11.00000 0.02259 0.03368 = 0.03460 0.01144 0.00040 -0.00078 O2 4 -0.670345 0.154915 0.077511 11.00000 0.02478 0.04424 = 0.04884 0.02666 -0.00666 0.00122 P1 5 -0.088398 0.180482 0.371245 11.00000 0.01958 0.02961 = 0.02234 0.00661 0.00180 0.00453 S1 6 0.005595 0.010005 0.304341 11.00000 0.02232 0.03167 = 0.01942 0.00496 0.00445 0.00657 S2 6 -0.116308 0.210749 0.535223 11.00000 0.02081 0.03487 = 0.02155 0.00570 0.00428 0.01034 NI1 8 0.000000 0.000000 0.500000 10.50000 0.01375 0.02915 = 0.01614 0.00329 0.00128 0.00512 MOLE 2 C10 1 0.155479 0.442212 0.098863 11.00000 0.02240 0.02802 = 0.02375 0.01075 0.00130 0.00443 C11 1 0.105788 0.331332 -0.019291 11.00000 0.02554 0.02816 = 0.02536 0.00893 0.00393 0.00384 AFIX 43 H11 2 0.167181 0.292198 -0.075190 11.00000 -1.20000 AFIX 0 C12 1 -0.050514 0.290217 -0.038307 11.00000 0.02903 0.02378 = 0.02686 0.00783 -0.00209 -0.00075 AFIX 43 H12 2 -0.112129 0.219113 -0.109305 11.00000 -1.20000 AFIX 0 C13 1 -0.099053 0.373194 0.066544 11.00000 0.02273 0.03430 = 0.03017 0.01476 0.00323 0.00013 AFIX 43 H13 2 -0.198954 0.366685 0.078043 11.00000 -1.20000 AFIX 0 C14 1 0.026267 0.467979 0.151934 11.00000 0.02856 0.02907 = 0.02417 0.01035 -0.00100 0.00259 AFIX 43 H14 2 0.024949 0.536005 0.229907 11.00000 -1.20000 AFIX 0 C15 1 0.308704 0.518410 0.147876 11.00000 0.02381 0.03219 = 0.02654 0.01214 0.00488 0.00964 AFIX 43 H15 2 0.378061 0.498159 0.096210 11.00000 -1.20000 AFIX 0 C16 1 0.357519 0.614257 0.260046 11.00000 0.02273 0.03356 = 0.02939 0.00952 0.00501 0.00634 AFIX 43 H16 2 0.287314 0.630962 0.310988 11.00000 -1.20000 AFIX 0 C17 1 0.508382 0.696862 0.313330 11.00000 0.01884 0.03216 = 0.02981 0.01364 0.00098 0.00587 C18 1 0.534098 0.807831 0.426802 11.00000 0.01766 0.03723 = 0.02972 0.00933 0.00446 0.00786 AFIX 43 H18 2 0.455157 0.827175 0.469292 11.00000 -1.20000 AFIX 0 C19 1 0.673603 0.889533 0.477525 11.00000 0.01904 0.03469 = 0.02579 0.00703 0.00314 0.00766 AFIX 43 H19 2 0.687548 0.965308 0.554587 11.00000 -1.20000 AFIX 0 C20 1 0.768554 0.758126 0.315432 11.00000 0.02180 0.03116 = 0.02168 0.00863 0.00398 0.00831 AFIX 43 H20 2 0.850774 0.738732 0.276740 11.00000 -1.20000 AFIX 0 C21 1 0.631394 0.672563 0.257952 11.00000 0.02756 0.02559 = 0.02134 0.00552 -0.00167 0.00278 AFIX 43 H21 2 0.620528 0.597346 0.180967 11.00000 -1.20000 AFIX 0 N1 3 0.791142 0.867660 0.423669 11.00000 0.01841 0.03108 = 0.02034 0.00661 0.00205 0.00632 FE1 7 0.000000 0.500000 0.000000 10.50000 0.01704 0.02274 = 0.01912 0.00496 -0.00100 0.00035 HKLF 4 Covalent radii and connectivity table for 2006slh0985 in P-1 C 0.770 H 0.320 N 0.700 O 0.660 P 1.100 S 1.030 FE 1.240 NI 1.250 C1 - C2 C6 P1 C2 - C1 C3 C3 - C4 C2 C4 - O2 C3 C5 C5 - C6 C4 C6 - C5 C1 C7 - O2 C8 - O1 C9 C9 - C8 O1 - C8 P1 O2 - C4 C7 P1 - O1 C1 S1 S2 S1 - P1 Ni1 S2 - P1 Ni1 Ni1 - N1_$4 N1_$5 S2_$1 S2 S1_$1 S1 C10 - C11 C14 C15 Fe1 C11 - C12 C10 Fe1 C12 - C13 C11 Fe1 C13 - C12 C14 Fe1 C14 - C13 C10 Fe1 C15 - C16 C10 C16 - C15 C17 C17 - C18 C21 C16 C18 - C19 C17 C19 - N1 C18 C20 - N1 C21 C21 - C20 C17 N1 - C19 C20 Ni1_$2 Fe1 - C13 C13_$3 C14_$3 C14 C12 C12_$3 C10_$3 C10 C11 C11_$3 Operators for generating equivalent atoms: $1 -x, -y, -z+1 $2 x+1, y+1, z $3 -x, -y+1, -z $4 x-1, y-1, z $5 -x+1, -y+1, -z+1 23772 Reflections read, of which 23 rejected -11 =< h =< 11, -13 =< k =< 13, -16 =< 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) 1 7 8 -42.01 20.27 2 105.50 1 Inconsistent equivalents 4939 Unique reflections, of which 0 suppressed R(int) = 0.0593 R(sigma) = 0.0575 Friedel opposites merged Maximum memory for data reduction = 2863 / 49298 Special position constraints for Ni1 x = 0.0000 y = 0.0000 z = 0.5000 sof = 0.50000 Input constraints retained (at least in part) for sof Special position constraints for Fe1 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 = 3593 / 325969 wR2 = 0.0955 before cycle 1 for 4939 data and 259 / 259 parameters GooF = S = 1.050; Restrained GooF = 1.050 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0337 * P )^2 + 0.93 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.71743 0.00123 -0.024 OSF 2 0.00478 0.00097 -0.004 EXTI Mean shift/esd = 0.008 Maximum = -0.045 for U11 Ni1 Max. shift = 0.000 A for H7B Max. dU = 0.000 for C9 Least-squares cycle 2 Maximum vector length = 511 Memory required = 3593 / 325969 wR2 = 0.0955 before cycle 2 for 4939 data and 259 / 259 parameters GooF = S = 1.050; Restrained GooF = 1.050 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0337 * P )^2 + 0.93 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.71741 0.00123 -0.013 OSF 2 0.00478 0.00097 -0.001 EXTI Mean shift/esd = 0.003 Maximum = -0.014 for U11 Ni1 Max. shift = 0.000 A for H7B Max. dU = 0.000 for C9 Least-squares cycle 3 Maximum vector length = 511 Memory required = 3593 / 325969 wR2 = 0.0955 before cycle 3 for 4939 data and 259 / 259 parameters GooF = S = 1.050; Restrained GooF = 1.050 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0337 * P )^2 + 0.93 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.71741 0.00123 0.000 OSF 2 0.00477 0.00097 -0.001 EXTI Mean shift/esd = 0.000 Maximum = 0.003 for U22 C9 Max. shift = 0.000 A for C9 Max. dU = 0.000 for C9 Least-squares cycle 4 Maximum vector length = 511 Memory required = 3593 / 325969 wR2 = 0.0955 before cycle 4 for 4939 data and 259 / 259 parameters GooF = S = 1.050; Restrained GooF = 1.050 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0337 * P )^2 + 0.93 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.71742 0.00123 0.001 OSF 2 0.00477 0.00097 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.001 for OSF Max. shift = 0.000 A for H7A Max. dU = 0.000 for C9 Least-squares cycle 5 Maximum vector length = 511 Memory required = 3593 / 325969 wR2 = 0.0955 before cycle 5 for 4939 data and 259 / 259 parameters GooF = S = 1.050; Restrained GooF = 1.050 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0337 * P )^2 + 0.93 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.71742 0.00123 0.001 OSF 2 0.00478 0.00097 0.001 EXTI Mean shift/esd = 0.000 Maximum = 0.001 for OSF Max. shift = 0.000 A for H9A Max. dU = 0.000 for C9 Least-squares cycle 6 Maximum vector length = 511 Memory required = 3593 / 325969 wR2 = 0.0955 before cycle 6 for 4939 data and 259 / 259 parameters GooF = S = 1.050; Restrained GooF = 1.050 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0337 * P )^2 + 0.93 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.71742 0.00123 0.000 OSF 2 0.00477 0.00097 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for EXTI Max. shift = 0.000 A for H9A Max. dU = 0.000 for C2 Largest correlation matrix elements 0.584 EXTI / OSF 0.522 U23 C7 / U22 C7 0.511 U23 C2 / U22 C2 0.556 U23 O2 / U33 O2 0.521 U23 C9 / U22 C9 0.511 U23 C5 / U22 C5 0.549 U23 O2 / U22 O2 0.517 U23 C3 / U33 C3 0.510 U23 C4 / U33 C4 0.536 U23 C9 / U33 C9 0.514 U23 C5 / U33 C5 0.525 U23 C7 / U33 C7 0.513 U23 C2 / U33 C2 Idealized hydrogen atom generation before cycle 7 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2 -0.3470 -0.0310 0.2471 43 0.950 0.000 C2 C1 C3 H3 -0.5794 -0.0473 0.1333 43 0.950 0.000 C3 C4 C2 H5 -0.4583 0.3541 0.1776 43 0.950 0.000 C5 C6 C4 H6 -0.2280 0.3691 0.2911 43 0.950 0.000 C6 C5 C1 H7A -0.7494 -0.0501 -0.0135 137 0.980 0.000 C7 O2 H7A H7B -0.8704 0.0476 -0.0178 137 0.980 0.000 C7 O2 H7A H7C -0.8218 0.0250 0.1004 137 0.980 0.000 C7 O2 H7A H8A 0.1671 0.3542 0.5075 23 0.990 0.000 C8 O1 C9 H8B 0.1579 0.4861 0.4756 23 0.990 0.000 C8 O1 C9 H9A 0.2675 0.2397 0.3423 137 0.980 0.000 C9 C8 H9A H9B 0.3642 0.3946 0.4161 137 0.980 0.000 C9 C8 H9A H9C 0.2440 0.3600 0.2977 137 0.980 0.000 C9 C8 H9A ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C11 ** H11 0.1672 0.2922 -0.0752 43 0.950 0.000 C11 C12 C10 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C12 ** H12 -0.1121 0.2191 -0.1093 43 0.950 0.000 C12 C13 C11 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C13 ** H13 -0.1990 0.3667 0.0780 43 0.950 0.000 C13 C12 C14 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C14 ** H14 0.0249 0.5360 0.2299 43 0.950 0.000 C14 C13 C10 H15 0.3781 0.4982 0.0962 43 0.950 0.000 C15 C16 C10 H16 0.2873 0.6310 0.3110 43 0.950 0.000 C16 C15 C17 H18 0.4552 0.8272 0.4693 43 0.950 0.000 C18 C19 C17 H19 0.6875 0.9653 0.5546 43 0.950 0.000 C19 N1 C18 H20 0.8508 0.7387 0.2767 43 0.950 0.000 C20 N1 C21 H21 0.6205 0.5973 0.1810 43 0.950 0.000 C21 C20 C17 2006slh0985 in P-1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 -0.26345 0.16941 0.27933 1.00000 0.02650 0.02995 0.02555 0.01102 0.00360 0.00716 0.02762 0.00623 0.00030 0.00029 0.00024 0.00000 0.00143 0.00154 0.00142 0.00125 0.00115 0.00118 0.00062 C2 -0.36939 0.04740 0.23258 1.00000 0.03078 0.03625 0.04276 0.01989 -0.00613 0.00628 0.03702 0.00678 0.00032 0.00033 0.00028 0.00000 0.00160 0.00174 0.00181 0.00151 0.00137 0.00132 0.00075 H2 -0.34701 -0.03096 0.24706 1.00000 0.04442 0.00000 0.00000 C3 -0.50805 0.03707 0.16480 1.00000 0.02941 0.03425 0.04398 0.01902 -0.00458 -0.00024 0.03684 0.00692 0.00033 0.00033 0.00028 0.00000 0.00158 0.00170 0.00184 0.00150 0.00136 0.00130 0.00074 H3 -0.57938 -0.04734 0.13329 1.00000 0.04421 0.00000 0.00000 C4 -0.54027 0.15191 0.14409 1.00000 0.02446 0.03815 0.03277 0.01713 -0.00009 0.00518 0.03178 0.00658 0.00031 0.00032 0.00026 0.00000 0.00145 0.00171 0.00158 0.00140 0.00122 0.00124 0.00067 C5 -0.43565 0.27547 0.19146 1.00000 0.03125 0.03366 0.04332 0.01929 -0.00022 0.00370 0.03610 0.00681 0.00033 0.00033 0.00028 0.00000 0.00160 0.00170 0.00181 0.00149 0.00136 0.00131 0.00072 H5 -0.45832 0.35414 0.17760 1.00000 0.04332 0.00000 0.00000 C6 -0.29868 0.28416 0.25869 1.00000 0.02900 0.03263 0.03394 0.01264 0.00125 0.00171 0.03321 0.00670 0.00032 0.00032 0.00026 0.00000 0.00153 0.00163 0.00162 0.00137 0.00127 0.00125 0.00069 H6 -0.22800 0.36908 0.29109 1.00000 0.03986 0.00000 0.00000 C7 -0.78723 0.03483 0.03314 1.00000 0.02299 0.04836 0.05052 0.02481 -0.00705 -0.00344 0.04168 0.00689 0.00032 0.00034 0.00030 0.00000 0.00151 0.00199 0.00201 0.00170 0.00139 0.00137 0.00081 H7A -0.74937 -0.05015 -0.01353 1.00000 0.06252 0.00000 0.00000 H7B -0.87044 0.04757 -0.01782 1.00000 0.06252 0.00000 0.00000 H7C -0.82181 0.02497 0.10042 1.00000 0.06252 0.00000 0.00000 C8 0.14995 0.38234 0.44084 1.00000 0.02617 0.04498 0.04081 0.01056 -0.00037 -0.00094 0.04124 0.00689 0.00032 0.00035 0.00029 0.00000 0.00157 0.00192 0.00183 0.00157 0.00136 0.00138 0.00080 H8A 0.16709 0.35415 0.50747 1.00000 0.04948 0.00000 0.00000 H8B 0.15786 0.48609 0.47560 1.00000 0.04948 0.00000 0.00000 C9 0.26636 0.34058 0.36800 1.00000 0.04076 0.07591 0.06004 0.03395 0.01108 0.00869 0.05725 0.00907 0.00039 0.00044 0.00035 0.00000 0.00201 0.00277 0.00242 0.00219 0.00177 0.00188 0.00101 H9A 0.26749 0.23970 0.34228 1.00000 0.08588 0.00000 0.00000 H9B 0.36418 0.39457 0.41610 1.00000 0.08588 0.00000 0.00000 H9C 0.24403 0.35999 0.29766 1.00000 0.08588 0.00000 0.00000 O1 0.00089 0.31671 0.36923 1.00000 0.02258 0.03367 0.03460 0.01144 0.00040 -0.00078 0.03235 0.00425 0.00020 0.00021 0.00017 0.00000 0.00099 0.00113 0.00111 0.00094 0.00084 0.00082 0.00047 O2 -0.67035 0.15491 0.07751 1.00000 0.02476 0.04424 0.04885 0.02667 -0.00668 0.00121 0.03890 0.00463 0.00021 0.00022 0.00019 0.00000 0.00105 0.00130 0.00132 0.00112 0.00094 0.00092 0.00053 P1 -0.08840 0.18048 0.37125 1.00000 0.01958 0.02961 0.02234 0.00661 0.00180 0.00452 0.02559 0.00156 0.00008 0.00008 0.00006 0.00000 0.00035 0.00040 0.00036 0.00032 0.00028 0.00029 0.00018 S1 0.00560 0.01000 0.30434 1.00000 0.02232 0.03166 0.01941 0.00496 0.00445 0.00657 0.02629 0.00151 0.00007 0.00007 0.00006 0.00000 0.00034 0.00039 0.00033 0.00030 0.00027 0.00028 0.00018 S2 -0.11631 0.21075 0.53522 1.00000 0.02080 0.03487 0.02155 0.00571 0.00428 0.01034 0.02745 0.00154 0.00007 0.00008 0.00006 0.00000 0.00034 0.00040 0.00034 0.00030 0.00027 0.00029 0.00018 Ni1 0.00000 0.00000 0.50000 0.50000 0.01374 0.02914 0.01614 0.00330 0.00128 0.00512 0.02189 0.00000 0.00000 0.00000 0.00000 0.00000 0.00023 0.00028 0.00024 0.00021 0.00018 0.00019 0.00014 C10 0.15548 0.44221 0.09887 1.00000 0.02236 0.02801 0.02376 0.01077 0.00130 0.00441 0.02517 0.00596 0.00029 0.00028 0.00023 0.00000 0.00136 0.00148 0.00136 0.00121 0.00109 0.00112 0.00060 C11 0.10579 0.33134 -0.01928 1.00000 0.02553 0.02815 0.02537 0.00894 0.00394 0.00387 0.02737 0.00607 0.00030 0.00029 0.00024 0.00000 0.00142 0.00151 0.00143 0.00123 0.00115 0.00116 0.00062 H11 0.16719 0.29221 -0.07518 1.00000 0.03285 0.00000 0.00000 C12 -0.05051 0.29022 -0.03830 1.00000 0.02900 0.02377 0.02683 0.00782 -0.00210 -0.00075 0.02878 0.00617 0.00030 0.00029 0.00025 0.00000 0.00149 0.00145 0.00146 0.00123 0.00119 0.00117 0.00064 H12 -0.11213 0.21912 -0.10930 1.00000 0.03453 0.00000 0.00000 C13 -0.09905 0.37319 0.06654 1.00000 0.02270 0.03429 0.03018 0.01477 0.00323 0.00013 0.02931 0.00618 0.00030 0.00030 0.00025 0.00000 0.00139 0.00161 0.00152 0.00133 0.00118 0.00119 0.00064 H13 -0.19895 0.36669 0.07804 1.00000 0.03517 0.00000 0.00000 C14 0.02627 0.46798 0.15193 1.00000 0.02859 0.02903 0.02416 0.01034 -0.00099 0.00260 0.02847 0.00619 0.00030 0.00030 0.00025 0.00000 0.00148 0.00152 0.00141 0.00124 0.00116 0.00119 0.00063 H14 0.02494 0.53600 0.22991 1.00000 0.03416 0.00000 0.00000 C15 0.30871 0.51842 0.14788 1.00000 0.02380 0.03218 0.02655 0.01214 0.00488 0.00963 0.02730 0.00620 0.00030 0.00029 0.00024 0.00000 0.00138 0.00156 0.00145 0.00128 0.00114 0.00117 0.00062 H15 0.37806 0.49816 0.09622 1.00000 0.03276 0.00000 0.00000 C16 0.35752 0.61425 0.26004 1.00000 0.02273 0.03355 0.02940 0.00954 0.00500 0.00633 0.02979 0.00621 0.00030 0.00030 0.00025 0.00000 0.00140 0.00162 0.00152 0.00132 0.00118 0.00120 0.00065 H16 0.28731 0.63095 0.31098 1.00000 0.03575 0.00000 0.00000 C17 0.50838 0.69687 0.31333 1.00000 0.01880 0.03217 0.02982 0.01366 0.00099 0.00587 0.02710 0.00618 0.00029 0.00030 0.00025 0.00000 0.00132 0.00153 0.00148 0.00129 0.00113 0.00113 0.00062 C18 0.53411 0.80783 0.42680 1.00000 0.01765 0.03719 0.02971 0.00932 0.00445 0.00785 0.02965 0.00622 0.00029 0.00030 0.00025 0.00000 0.00131 0.00165 0.00150 0.00132 0.00113 0.00117 0.00065 H18 0.45516 0.82717 0.46929 1.00000 0.03558 0.00000 0.00000 C19 0.67360 0.88953 0.47752 1.00000 0.01904 0.03467 0.02579 0.00703 0.00314 0.00768 0.02839 0.00628 0.00029 0.00030 0.00025 0.00000 0.00134 0.00161 0.00142 0.00128 0.00111 0.00116 0.00064 H19 0.68754 0.96531 0.55458 1.00000 0.03407 0.00000 0.00000 C20 0.76856 0.75813 0.31543 1.00000 0.02180 0.03114 0.02169 0.00865 0.00398 0.00832 0.02552 0.00591 0.00029 0.00028 0.00023 0.00000 0.00134 0.00153 0.00135 0.00121 0.00109 0.00115 0.00060 H20 0.85078 0.73873 0.27674 1.00000 0.03062 0.00000 0.00000 C21 0.63139 0.67256 0.25795 1.00000 0.02755 0.02556 0.02133 0.00552 -0.00167 0.00278 0.02718 0.00602 0.00030 0.00029 0.00024 0.00000 0.00146 0.00146 0.00134 0.00119 0.00113 0.00115 0.00062 H21 0.62052 0.59734 0.18097 1.00000 0.03261 0.00000 0.00000 N1 0.79114 0.86766 0.42367 1.00000 0.01840 0.03106 0.02032 0.00661 0.00206 0.00634 0.02477 0.00483 0.00023 0.00023 0.00019 0.00000 0.00110 0.00128 0.00112 0.00101 0.00090 0.00094 0.00051 Fe1 0.00000 0.50000 0.00000 0.50000 0.01703 0.02274 0.01911 0.00496 -0.00100 0.00035 0.02170 0.00000 0.00000 0.00000 0.00000 0.00000 0.00027 0.00029 0.00027 0.00023 0.00021 0.00021 0.00015 Final Structure Factor Calculation for 2006slh0985 in P-1 Total number of l.s. parameters = 259 Maximum vector length = 511 Memory required = 3334 / 27083 wR2 = 0.0955 before cycle 7 for 4939 data and 0 / 259 parameters GooF = S = 1.050; Restrained GooF = 1.050 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0337 * P )^2 + 0.93 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0421 for 3569 Fo > 4sig(Fo) and 0.0734 for all 4939 data wR2 = 0.0955, GooF = S = 1.050, Restrained GooF = 1.050 for all data Occupancy sum of asymmetric unit = 28.00 for non-hydrogen and 22.00 for hydrogen atoms Principal mean square atomic displacements U 0.0326 0.0266 0.0236 C1 0.0551 0.0358 0.0202 C2 0.0540 0.0319 0.0247 C3 0.0392 0.0351 0.0211 C4 0.0491 0.0313 0.0279 C5 0.0384 0.0350 0.0262 C6 0.0630 0.0429 0.0191 C7 0.0567 0.0435 0.0235 C8 0.0767 0.0547 0.0403 C9 0.0397 0.0369 0.0205 O1 0.0610 0.0363 0.0195 O2 0.0354 0.0228 0.0186 P1 0.0388 0.0219 0.0182 S1 0.0437 0.0214 0.0172 S2 0.0369 0.0159 0.0129 Ni1 0.0287 0.0271 0.0197 C10 0.0315 0.0265 0.0241 C11 0.0377 0.0293 0.0194 C12 0.0372 0.0291 0.0216 C13 0.0347 0.0301 0.0207 C14 0.0348 0.0266 0.0205 C15 0.0390 0.0282 0.0222 C16 0.0324 0.0320 0.0169 C17 0.0438 0.0287 0.0164 C18 0.0427 0.0246 0.0178 C19 0.0352 0.0217 0.0197 C20 0.0352 0.0285 0.0178 C21 0.0366 0.0206 0.0171 N1 0.0283 0.0231 0.0137 Fe1 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.016 0.029 0.046 0.062 0.080 0.101 0.127 0.163 0.226 1.000 Number in group 525. 468. 511. 490. 478. 493. 493. 494. 489. 498. GooF 0.894 0.955 1.066 1.042 1.167 1.075 1.064 1.137 0.954 1.125 K 1.361 0.994 0.886 0.941 0.933 0.977 0.982 0.997 1.017 1.011 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.05 1.15 1.31 1.65 inf Number in group 498. 502. 485. 489. 504. 496. 481. 494. 494. 496. GooF 0.963 0.989 0.999 0.954 1.012 1.009 0.958 0.960 1.052 1.493 K 0.978 0.980 1.001 0.994 1.005 1.011 1.023 1.018 1.010 0.997 R1 0.215 0.171 0.139 0.097 0.079 0.060 0.046 0.035 0.030 0.029 Recommended weighting scheme: WGHT 0.0336 0.9297 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) -2 0 3 273.01 439.63 6.85 0.146 3.20 1 0 1 51.05 129.83 5.97 0.079 6.40 0 2 0 81.46 40.70 5.03 0.044 4.74 -2 2 1 78.38 37.95 5.01 0.043 3.26 1 1 0 82.99 144.56 4.90 0.084 6.01 0 1 2 224.41 150.15 4.89 0.085 4.11 2 9 3 49.57 126.81 4.37 0.078 0.87 0 3 0 248.08 337.74 4.24 0.128 3.16 0 -4 1 4.01 32.14 4.01 0.039 2.55 1 -2 3 31.15 10.24 3.96 0.022 3.44 0 2 1 691.57 847.21 3.87 0.203 3.82 -2 -5 2 306.53 233.82 3.67 0.106 1.81 4 -1 10 -7.64 14.49 3.63 0.026 0.97 3 -1 1 162.29 116.02 3.44 0.075 2.85 -1 -4 6 80.74 49.11 3.43 0.049 1.90 3 -1 3 6.91 24.93 3.38 0.035 2.27 -1 1 2 3818.48 4375.21 3.32 0.460 4.10 2 5 0 145.86 104.76 3.18 0.071 1.65 -1 0 4 445.84 539.40 3.17 0.162 2.84 0 9 4 -14.87 28.55 3.13 0.037 0.87 6 2 8 478.32 349.38 3.13 0.130 0.85 -4 10 3 -3.60 67.69 3.10 0.057 0.84 2 5 8 -28.82 37.64 3.08 0.043 0.89 -1 -1 3 90.41 53.57 3.06 0.051 3.97 -4 3 2 63.09 97.69 3.04 0.069 1.83 6 -8 2 70.09 116.83 3.04 0.075 1.05 -1 6 1 16.29 40.59 3.04 0.044 1.51 6 5 5 25.64 84.15 3.04 0.064 0.85 3 -2 2 329.88 408.86 3.03 0.141 2.53 -9 9 0 49.32 123.47 3.03 0.077 0.80 -7 1 12 -37.54 126.25 3.03 0.078 0.82 0 -6 7 166.82 117.77 3.00 0.076 1.48 3 4 7 343.03 478.67 2.99 0.152 0.98 0 -1 2 340.95 414.56 2.97 0.142 6.09 6 -11 1 169.77 284.93 2.94 0.118 0.83 -4 -9 3 45.97 84.65 2.94 0.064 0.97 0 -3 1 23.96 9.07 2.92 0.021 3.45 1 -3 10 47.23 19.89 2.87 0.031 1.20 -2 2 5 1737.55 1524.26 2.84 0.272 1.77 -8 -3 1 248.17 314.15 2.82 0.123 1.03 -2 1 2 3111.96 3515.98 2.79 0.413 3.44 4 2 10 189.67 287.50 2.77 0.118 0.85 4 6 6 1592.35 1332.50 2.77 0.254 0.85 -5 5 11 778.71 580.48 2.77 0.168 0.77 -9 2 3 324.21 236.79 2.75 0.107 1.00 -7 2 8 -0.23 31.44 2.74 0.039 0.99 3 -2 6 266.73 213.48 2.73 0.102 1.59 -2 -4 1 396.92 332.91 2.72 0.127 2.09 4 -13 5 291.82 165.80 2.71 0.090 0.79 -2 -12 6 12.86 78.23 2.70 0.062 0.84 Bond lengths and angles C1 - Distance Angles C2 1.3865 (0.0040) C6 1.3941 (0.0041) 118.58 (0.26) P1 1.8032 (0.0027) 120.01 (0.22) 121.34 (0.21) C1 - C2 C6 C2 - Distance Angles C1 1.3865 (0.0040) C3 1.3946 (0.0039) 121.52 (0.28) C2 - C1 C3 - Distance Angles C4 1.3876 (0.0041) C2 1.3946 (0.0039) 119.01 (0.27) C3 - C4 C4 - Distance Angles O2 1.3674 (0.0032) C3 1.3876 (0.0041) 124.96 (0.26) C5 1.3908 (0.0040) 114.94 (0.26) 120.10 (0.26) C4 - O2 C3 C5 - Distance Angles C6 1.3835 (0.0040) C4 1.3908 (0.0040) 120.20 (0.28) C5 - C6 C6 - Distance Angles C5 1.3835 (0.0040) C1 1.3941 (0.0041) 120.59 (0.27) C6 - C5 C7 - Distance Angles O2 1.4332 (0.0034) C7 - C8 - Distance Angles O1 1.4550 (0.0033) C9 1.4886 (0.0047) 111.41 (0.27) C8 - O1 C9 - Distance Angles C8 1.4886 (0.0047) C9 - O1 - Distance Angles C8 1.4550 (0.0033) P1 1.5930 (0.0021) 122.01 (0.20) O1 - C8 O2 - Distance Angles C4 1.3674 (0.0032) C7 1.4332 (0.0034) 117.89 (0.23) O2 - C4 P1 - Distance Angles O1 1.5930 (0.0021) C1 1.8032 (0.0027) 98.45 (0.12) S1 1.9934 (0.0010) 113.32 (0.08) 113.40 (0.10) S2 2.0016 (0.0010) 112.62 (0.08) 110.38 (0.10) 108.46 (0.05) P1 - O1 C1 S1 S1 - Distance Angles P1 1.9934 (0.0010) Ni1 2.4986 (0.0007) 84.70 (0.03) S1 - P1 S2 - Distance Angles P1 2.0016 (0.0010) Ni1 2.4679 (0.0007) 85.35 (0.03) S2 - P1 Ni1 - Distance Angles N1_$4 2.0994 (0.0021) N1_$5 2.0994 (0.0021) 180.00 S2_$1 2.4679 (0.0007) 88.85 (0.06) 91.15 (0.06) S2 2.4679 (0.0007) 91.15 (0.06) 88.85 (0.06) 180.00 S1_$1 2.4986 (0.0007) 91.18 (0.06) 88.82 (0.06) 81.48 (0.02) 98.52 (0.02) S1 2.4986 (0.0007) 88.82 (0.06) 91.18 (0.06) 98.52 (0.02) 81.48 (0.02) 180.00 Ni1 - N1_$4 N1_$5 S2_$1 S2 S1_$1 C10 - Distance Angles C11 1.4340 (0.0037) C14 1.4384 (0.0039) 107.22 (0.23) C15 1.4610 (0.0036) 124.20 (0.25) 128.42 (0.24) Fe1 2.0554 (0.0026) 69.65 (0.15) 69.13 (0.15) 122.84 (0.20) C10 - C11 C14 C15 C11 - Distance Angles C12 1.4160 (0.0038) C10 1.4340 (0.0037) 108.26 (0.24) Fe1 2.0571 (0.0028) 69.63 (0.16) 69.53 (0.16) C11 - C12 C10 C12 - Distance Angles C13 1.4132 (0.0040) C11 1.4160 (0.0038) 108.22 (0.24) Fe1 2.0516 (0.0027) 69.61 (0.16) 70.05 (0.16) C12 - C13 C11 C13 - Distance Angles C12 1.4132 (0.0040) C14 1.4211 (0.0037) 108.73 (0.25) Fe1 2.0459 (0.0028) 70.04 (0.16) 69.69 (0.16) C13 - C12 C14 C14 - Distance Angles C13 1.4211 (0.0037) C10 1.4384 (0.0039) 107.57 (0.25) Fe1 2.0462 (0.0028) 69.67 (0.16) 69.81 (0.16) C14 - C13 C10 C15 - Distance Angles C16 1.3299 (0.0038) C10 1.4610 (0.0036) 124.33 (0.26) C15 - C16 C16 - Distance Angles C15 1.3299 (0.0038) C17 1.4667 (0.0036) 126.82 (0.27) C16 - C15 C17 - Distance Angles C18 1.3925 (0.0038) C21 1.4007 (0.0039) 116.49 (0.24) C16 1.4667 (0.0036) 118.95 (0.25) 124.56 (0.25) C17 - C18 C21 C18 - Distance Angles C19 1.3761 (0.0037) C17 1.3925 (0.0038) 120.15 (0.26) C18 - C19 C19 - Distance Angles N1 1.3440 (0.0034) C18 1.3761 (0.0037) 123.39 (0.25) C19 - N1 C20 - Distance Angles N1 1.3459 (0.0033) C21 1.3817 (0.0036) 123.08 (0.25) C20 - N1 C21 - Distance Angles C20 1.3817 (0.0036) C17 1.4007 (0.0039) 119.92 (0.25) C21 - C20 N1 - Distance Angles C19 1.3440 (0.0034) C20 1.3459 (0.0033) 116.93 (0.23) Ni1_$2 2.0994 (0.0021) 122.44 (0.17) 120.60 (0.18) N1 - C19 C20 Fe1 - Distance Angles C13 2.0459 (0.0028) C13_$3 2.0459 (0.0028) 180.00 (0.12) C14_$3 2.0462 (0.0028) 139.36 (0.10) 40.64 (0.10) C14 2.0462 (0.0028) 40.64 (0.10) 139.36 (0.10) 180.00 (0.15) C12 2.0516 (0.0027) 40.35 (0.11) 139.65 (0.11) 111.59 (0.11) 68.41 (0.11) C12_$3 2.0516 (0.0027) 139.65 (0.11) 40.35 (0.11) 68.41 (0.11) 111.59 (0.11) 180.00 (0.17) C10_$3 2.0554 (0.0026) 111.54 (0.11) 68.46 (0.11) 41.06 (0.11) 138.94 (0.11) 111.57 (0.10) 68.43 (0.10) C10 2.0554 (0.0026) 68.46 (0.11) 111.54 (0.11) 138.94 (0.11) 41.06 (0.11) 68.43 (0.10) 111.57 (0.10) 180.00 (0.13) C11 2.0571 (0.0028) 67.92 (0.11) 112.08 (0.12) 111.40 (0.11) 68.60 (0.11) 40.32 (0.11) 139.68 (0.11) 139.18 (0.10) C11_$3 2.0571 (0.0028) 112.08 (0.12) 67.92 (0.12) 68.60 (0.11) 111.40 (0.11) 139.68 (0.11) 40.32 (0.11) 40.82 (0.10) Fe1 - C13 C13_$3 C14_$3 C14 C12 C12_$3 C10_$3 FMAP and GRID set by program FMAP 2 3 34 GRID -1.613 -2 -2 1.613 2 2 R1 = 0.0716 for 4939 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.61 at 0.2390 0.4554 0.4147 [ 1.12 A from H8B ] Deepest hole -0.45 at 0.9414 0.1787 0.3154 [ 0.78 A from P1 ] Mean = 0.00, Rms deviation from mean = 0.08 e/A^3, Highest memory used = 3199 / 25852 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.2390 0.4554 0.4147 1.00000 0.05 0.61 1.12 H8B 1.18 C9 1.24 C8 1.37 H9B Q2 1 0.1451 0.4106 0.5325 1.00000 0.05 0.45 0.62 H8A 1.07 C8 1.27 H8B 2.06 O1 Q3 1 0.0887 0.3250 0.1280 1.00000 0.05 0.45 1.52 C10 1.60 C14 1.90 C11 1.99 C13 Q4 1 0.1389 0.3684 0.0504 1.00000 0.05 0.44 0.75 C10 0.79 C11 1.52 H11 1.82 C14 Q5 1 0.2583 0.5821 0.2194 1.00000 0.05 0.42 0.93 C16 1.03 H16 1.08 C15 1.69 C10 Shortest distances between peaks (including symmetry equivalents) 3 4 1.34 1 2 2.00 4 5 2.39 3 5 2.69 Time profile in seconds ----------------------- 0.09: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.01: Generate connectivity array 0.03: 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. 7.23: Read intensity data, sort/merge etc. 0.01: Set up constraints 0.01: OSF, H-atoms from difference map 0.02: Set up l.s. refinement 0.00: Generate idealized H-atoms 3.83: Structure factors and derivatives 6.95: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.05: Apply other restraints 1.11: Solve l.s. equations 0.00: Generate HTAB table 0.07: Other dependent quantities, CIF, tables 0.19: Analysis of variance 0.07: Merge reflections for Fourier and .fcf 0.16: Fourier summations 0.05: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2006slh0985 finished at 12:18:05 Total CPU time: 19.9 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++