+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL - CRYSTAL STRUCTURE REFINEMENT - MULTI-CPU VERSION + + Copyright(C) George M. Sheldrick 1993-2016 Version 2016/6 + + shelx started at 17:27:09 on 04-Apr-2017 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Command line parameters: shelx -a50000 -b3000 -c624 -g0 -m0 -t4 -a sets the approximate maximum number of atoms including hydrogens. -b sets the maximum number of full-matrix parameters (not used by CGLS). For example -b9000 allows refinement of 1000 anisotropic atoms or 3000 with BLOC 1. For a 32-bit version, -b times the square root of the number of threads should not exceed about 65500. -c sets the reflection buffer size. This depends on the CPU cache size but will rarely need changing. -g sets the number of reflection groups used for calculating R_complete, This must be greater than 1 but not greater than the total number of reflections for refinement. -m sets the current reflection group number. This may not be less than 1 nor greater than the number set by -g. These command line flags override other ways of defining free-R reflections. The -m value is also used as a seed for the WIGL pseudo-random shifts. -t sets the number of threads, otherwise it is set to the apparent number of CPUs. For optimal performance on hyperthreading systems, -t should be set to a little more than half the number of CPUs; e.g. -t4 or -t5 for an Intel i7 processor. Running 4 threads on 4 processors Covalent radii and connectivity table for NiClMelDMF C 0.770 H 0.320 N 0.700 O 0.660 CL 0.990 NI 1.250 Ni1 - O21 O21_$1 O41 O1 O31 Cl2 Cl2 - Ni1 Cl3 - no bonds found N11 - C16 C12 C12 - N12 N13 N11 N12 - C12 N13 - C14 C12 C14 - N13 N15 N14 N14 - C14 N15 - C16 C14 C16 - N15 N11 N16 N16 - C16 O21 - C22 Ni1 C22 - O21 N23 N23 - C22 C25 C24 C24 - N23 C25 - N23 O31 - C32 Ni1 C32 - O31 N33 N33 - C32 C35 C34 C34 - N33 C35 - N33 O41 - C42 Ni1 C42 - O41 N43 N43 - C42 C44 C45 C44 - N43 C45 - N43 O1 - Ni1 Operators for generating equivalent atoms: $1 x, -y+1/2, z 10356 Reflections read, of which 0 rejected -26 =< h =< 26, -23 =< k =< 23, -17 =< l =< 17, Max. 2-theta = 60.05 0 Systematic absence violations (I>3sig(I)) before merging 10 Inconsistent equivalents 5733 Unique reflections, of which 0 suppressed R(int) = 0.0198 R(sigma) = 0.0273 Friedel opposites merged Maximum memory for data reduction = 1696 / 56964 Number of data for d > 0.710A (CIF: max) and d > 0.833A (CIF: full) (ignoring systematic absences): Unique reflections found (point group) 5733 3562 Unique reflections possible (point group) 5736 3563 Unique reflections found (Laue group) 5733 3562 Unique reflections possible (Laue group) 5736 3563 Special position constraints for Ni1 y = 0.2500 U23 = 0 U12 = 0 sof = 0.50000 Input constraints retained (at least in part) for xyz and sof Special position constraints for Cl2 y = 0.2500 U23 = 0 U12 = 0 sof = 0.50000 Input constraints retained (at least in part) for sof Special position constraints for Cl3 y = 0.2500 U23 = 0 U12 = 0 sof = 0.50000 Input constraints retained (at least in part) for xyz and sof Special position constraints for O31 y = 0.2500 U23 = 0 U12 = 0 sof = 0.50000 Input constraints retained (at least in part) for xyz and sof Special position constraints for C32 y = 0.2500 U23 = 0 U12 = 0 sof = 0.50000 Input constraints retained (at least in part) for xyz and sof Special position constraints for N33 y = 0.2500 U23 = 0 U12 = 0 sof = 0.50000 Input constraints retained (at least in part) for xyz and sof Special position constraints for C34 y = 0.2500 U23 = 0 U12 = 0 sof = 0.50000 Input constraints retained (at least in part) for sof Special position constraints for C35 y = 0.2500 U23 = 0 U12 = 0 sof = 0.50000 Input constraints retained (at least in part) for sof Special position constraints for O41 y = 0.2500 U23 = 0 U12 = 0 sof = 0.50000 Input constraints retained (at least in part) for xyz and sof Special position constraints for C42 y = 0.2500 U23 = 0 U12 = 0 sof = 0.50000 Input constraints retained (at least in part) for xyz and sof Special position constraints for N43 y = 0.2500 U23 = 0 U12 = 0 sof = 0.50000 Input constraints retained (at least in part) for xyz and sof Special position constraints for C44 y = 0.2500 U23 = 0 U12 = 0 sof = 0.50000 Input constraints retained (at least in part) for xyz and sof Special position constraints for C45 y = 0.2500 U23 = 0 U12 = 0 sof = 0.50000 Input constraints retained (at least in part) for sof Special position constraints for O1 y = 0.2500 U23 = 0 U12 = 0 sof = 0.50000 Input constraints retained (at least in part) for xyz and sof ** Cell contents from UNIT instruction and atom list do not agree ** Unit-cell contents from UNIT instruction and atom list resp. C 72.00 72.00 H 176.00 0.00 N 64.00 64.00 O 24.00 20.00 CL 8.00 8.00 NI 4.00 4.00 Least-squares cycle 1 Maximum vector length = 623 Memory required = 41 / 2243 / 316221 wR2 = 0.2962 before cycle 1 for 5733 data and 211 / 211 parameters GooF = S = 1.118; Restrained GooF = 1.118 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1918 * P )^2 + 2.36 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.58548 0.00266 -0.017 OSF Mean shift/esd = 0.026 Maximum = -0.110 for x N43 Max. shift = 0.003 A for C35 Max. dU =-0.001 for C45 Least-squares cycle 2 Maximum vector length = 623 Memory required = 41 / 2243 / 316221 wR2 = 0.2961 before cycle 2 for 5733 data and 211 / 211 parameters GooF = S = 1.118; Restrained GooF = 1.118 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1918 * P )^2 + 2.36 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.58552 0.00266 0.016 OSF Mean shift/esd = 0.014 Maximum = -0.068 for x N43 Max. shift = 0.001 A for C35 Max. dU =-0.002 for C45 Least-squares cycle 3 Maximum vector length = 623 Memory required = 41 / 2243 / 316221 wR2 = 0.2961 before cycle 3 for 5733 data and 211 / 211 parameters GooF = S = 1.118; Restrained GooF = 1.118 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1918 * P )^2 + 2.36 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.58553 0.00266 0.006 OSF Mean shift/esd = 0.005 Maximum = -0.035 for U22 C45 Max. shift = 0.000 A for C35 Max. dU =-0.001 for C45 Least-squares cycle 4 Maximum vector length = 623 Memory required = 41 / 2243 / 316221 wR2 = 0.2961 before cycle 4 for 5733 data and 211 / 211 parameters GooF = S = 1.118; Restrained GooF = 1.118 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1918 * P )^2 + 2.36 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.58554 0.00266 0.002 OSF Mean shift/esd = 0.003 Maximum = -0.019 for U22 C45 Max. shift = 0.000 A for C45 Max. dU =-0.001 for C45 Least-squares cycle 5 Maximum vector length = 623 Memory required = 41 / 2243 / 316221 wR2 = 0.2961 before cycle 5 for 5733 data and 211 / 211 parameters GooF = S = 1.118; Restrained GooF = 1.118 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1918 * P )^2 + 2.36 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.58555 0.00266 0.001 OSF Mean shift/esd = 0.002 Maximum = -0.012 for U22 C45 Max. shift = 0.000 A for C35 Max. dU = 0.000 for C45 Least-squares cycle 6 Maximum vector length = 623 Memory required = 41 / 2243 / 316221 wR2 = 0.2961 before cycle 6 for 5733 data and 211 / 211 parameters GooF = S = 1.118; Restrained GooF = 1.118 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1918 * P )^2 + 2.36 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.58555 0.00266 0.001 OSF Mean shift/esd = 0.001 Maximum = -0.007 for U22 C45 Max. shift = 0.000 A for C35 Max. dU = 0.000 for C45 Least-squares cycle 7 Maximum vector length = 623 Memory required = 41 / 2243 / 316221 wR2 = 0.2961 before cycle 7 for 5733 data and 211 / 211 parameters GooF = S = 1.118; Restrained GooF = 1.118 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1918 * P )^2 + 2.36 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.58555 0.00266 0.000 OSF Mean shift/esd = 0.001 Maximum = -0.004 for U22 C45 Max. shift = 0.000 A for C35 Max. dU = 0.000 for C45 Least-squares cycle 8 Maximum vector length = 623 Memory required = 41 / 2243 / 316221 wR2 = 0.2961 before cycle 8 for 5733 data and 211 / 211 parameters GooF = S = 1.118; Restrained GooF = 1.118 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1918 * P )^2 + 2.36 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.58555 0.00266 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.002 for U22 C45 Max. shift = 0.000 A for C35 Max. dU = 0.000 for C45 Least-squares cycle 9 Maximum vector length = 623 Memory required = 41 / 2243 / 316221 wR2 = 0.2961 before cycle 9 for 5733 data and 211 / 211 parameters GooF = S = 1.118; Restrained GooF = 1.118 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1918 * P )^2 + 2.36 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.58555 0.00266 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.001 for U22 C45 Max. shift = 0.000 A for C35 Max. dU = 0.000 for C45 Least-squares cycle 10 Maximum vector length = 623 Memory required = 41 / 2243 / 316221 wR2 = 0.2961 before cycle 10 for 5733 data and 211 / 211 parameters GooF = S = 1.118; Restrained GooF = 1.118 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1918 * P )^2 + 2.36 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.58555 0.00266 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.001 for x N43 Max. shift = 0.000 A for C35 Max. dU = 0.000 for C45 Least-squares cycle 11 Maximum vector length = 623 Memory required = 41 / 2243 / 316221 wR2 = 0.2961 before cycle 11 for 5733 data and 211 / 211 parameters GooF = S = 1.118; Restrained GooF = 1.118 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1918 * P )^2 + 2.36 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.58555 0.00266 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for U22 C45 Max. shift = 0.000 A for C45 Max. dU = 0.000 for C45 Least-squares cycle 12 Maximum vector length = 623 Memory required = 41 / 2243 / 316221 wR2 = 0.2961 before cycle 12 for 5733 data and 211 / 211 parameters GooF = S = 1.118; Restrained GooF = 1.118 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1918 * P )^2 + 2.36 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.58555 0.00266 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x N43 Max. shift = 0.000 A for C45 Max. dU = 0.000 for C45 Least-squares cycle 13 Maximum vector length = 623 Memory required = 41 / 2243 / 316221 wR2 = 0.2961 before cycle 13 for 5733 data and 211 / 211 parameters GooF = S = 1.118; Restrained GooF = 1.118 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1918 * P )^2 + 2.36 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.58555 0.00266 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x Ni1 Max. shift = 0.000 A for C45 Max. dU = 0.000 for C45 Least-squares cycle 14 Maximum vector length = 623 Memory required = 41 / 2243 / 316221 wR2 = 0.2961 before cycle 14 for 5733 data and 211 / 211 parameters GooF = S = 1.118; Restrained GooF = 1.118 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1918 * P )^2 + 2.36 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.58555 0.00266 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x Ni1 Max. shift = 0.000 A for C45 Max. dU = 0.000 for C45 Least-squares cycle 15 Maximum vector length = 623 Memory required = 41 / 2243 / 316221 wR2 = 0.2961 before cycle 15 for 5733 data and 211 / 211 parameters GooF = S = 1.118; Restrained GooF = 1.118 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1918 * P )^2 + 2.36 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.58555 0.00266 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x Ni1 Max. shift = 0.000 A for C35 Max. dU = 0.000 for C45 Least-squares cycle 16 Maximum vector length = 623 Memory required = 41 / 2243 / 316221 wR2 = 0.2961 before cycle 16 for 5733 data and 211 / 211 parameters GooF = S = 1.118; Restrained GooF = 1.118 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1918 * P )^2 + 2.36 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.58555 0.00266 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x Ni1 Max. shift = 0.000 A for C34 Max. dU = 0.000 for C45 Least-squares cycle 17 Maximum vector length = 623 Memory required = 41 / 2243 / 316221 wR2 = 0.2961 before cycle 17 for 5733 data and 211 / 211 parameters GooF = S = 1.118; Restrained GooF = 1.118 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1918 * P )^2 + 2.36 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.58555 0.00266 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x Ni1 Max. shift = 0.000 A for C45 Max. dU = 0.000 for C45 Least-squares cycle 18 Maximum vector length = 623 Memory required = 41 / 2243 / 316221 wR2 = 0.2961 before cycle 18 for 5733 data and 211 / 211 parameters GooF = S = 1.118; Restrained GooF = 1.118 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1918 * P )^2 + 2.36 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.58555 0.00266 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x Ni1 Max. shift = 0.000 A for N13 Max. dU = 0.000 for C45 Least-squares cycle 19 Maximum vector length = 623 Memory required = 41 / 2243 / 316221 wR2 = 0.2961 before cycle 19 for 5733 data and 211 / 211 parameters GooF = S = 1.118; Restrained GooF = 1.118 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1918 * P )^2 + 2.36 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.58555 0.00266 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x Ni1 Max. shift = 0.000 A for N33 Max. dU = 0.000 for C45 Least-squares cycle 20 Maximum vector length = 623 Memory required = 41 / 2243 / 316221 wR2 = 0.2961 before cycle 20 for 5733 data and 211 / 211 parameters GooF = S = 1.118; Restrained GooF = 1.118 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1918 * P )^2 + 2.36 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.58555 0.00266 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x Ni1 Max. shift = 0.000 A for N13 Max. dU = 0.000 for C35 Largest correlation matrix elements -0.735 U13 C35 / U33 C35 0.624 U13 C45 / U11 C45 0.569 z C45 / x C45 -0.726 U13 C35 / U11 C35 -0.620 U13 C32 / U11 C32 0.545 U11 Ni1 / OSF -0.690 U13 N33 / U33 N33 -0.602 U13 C32 / U33 C32 0.535 U33 Ni1 / OSF -0.685 U13 N33 / U11 N33 -0.591 z C35 / x C35 0.534 U22 Ni1 / OSF 0.657 U13 C45 / U33 C45 -0.581 z N33 / x N33 -0.513 z C32 / x C32 NiClMelDMF ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq Ni1 0.57507 0.25000 0.02003 0.50000 0.04064 0.02977 0.04136 0.00000 0.00011 0.00000 0.03726 0.00087 0.00003 0.00000 0.00005 0.00000 0.00036 0.00033 0.00036 0.00000 0.00022 0.00000 0.00022 Cl2 0.65695 0.25000 -0.13255 0.50000 0.06303 0.03055 0.03149 0.00000 0.00457 0.00000 0.04169 0.00176 0.00007 0.00000 0.00009 0.00000 0.00071 0.00049 0.00049 0.00000 0.00044 0.00000 0.00029 Cl3 0.63598 0.25000 0.46471 0.50000 0.09984 0.03670 0.04244 0.00000 -0.00338 0.00000 0.05966 0.00235 0.00010 0.00000 0.00012 0.00000 0.00120 0.00062 0.00065 0.00000 0.00065 0.00000 0.00042 N11 0.73562 0.39356 0.15371 1.00000 0.05123 0.02807 0.02934 -0.00099 -0.00307 -0.00596 0.03621 0.00428 0.00015 0.00015 0.00020 0.00000 0.00146 0.00112 0.00112 0.00091 0.00101 0.00101 0.00056 C12 0.73568 0.43851 0.24639 1.00000 0.04545 0.03315 0.02629 0.00072 -0.00247 -0.00458 0.03496 0.00504 0.00017 0.00018 0.00023 0.00000 0.00155 0.00134 0.00117 0.00107 0.00108 0.00113 0.00060 N12 0.71259 0.40351 0.33817 1.00000 0.08447 0.04407 0.03124 0.00459 0.00418 -0.02272 0.05326 0.00545 0.00021 0.00020 0.00023 0.00000 0.00230 0.00156 0.00127 0.00117 0.00137 0.00157 0.00082 N13 0.75833 0.51578 0.25300 1.00000 0.06024 0.03030 0.02376 -0.00087 -0.00165 -0.00963 0.03810 0.00436 0.00015 0.00016 0.00019 0.00000 0.00166 0.00115 0.00102 0.00091 0.00103 0.00108 0.00059 C14 0.78060 0.54765 0.15840 1.00000 0.05155 0.02880 0.02632 -0.00104 -0.00374 -0.00794 0.03556 0.00486 0.00017 0.00018 0.00023 0.00000 0.00163 0.00129 0.00120 0.00101 0.00112 0.00120 0.00062 N14 0.80415 0.62485 0.15951 1.00000 0.10366 0.03276 0.03438 -0.00619 0.00533 -0.02493 0.05693 0.00542 0.00023 0.00017 0.00024 0.00000 0.00264 0.00139 0.00132 0.00109 0.00158 0.00159 0.00090 N15 0.78044 0.50992 0.06052 1.00000 0.05867 0.03199 0.02397 -0.00184 -0.00057 -0.01034 0.03821 0.00438 0.00016 0.00016 0.00019 0.00000 0.00157 0.00117 0.00103 0.00093 0.00104 0.00112 0.00058 C16 0.75801 0.43304 0.06424 1.00000 0.04631 0.02982 0.02680 -0.00179 -0.00451 -0.00232 0.03431 0.00498 0.00017 0.00018 0.00023 0.00000 0.00156 0.00128 0.00120 0.00102 0.00109 0.00113 0.00060 N16 0.75948 0.39129 -0.03146 1.00000 0.07601 0.03580 0.03290 -0.01006 -0.00070 -0.00968 0.04824 0.00513 0.00020 0.00018 0.00023 0.00000 0.00214 0.00139 0.00130 0.00109 0.00129 0.00138 0.00075 O21 0.57484 0.37282 0.03464 1.00000 0.06423 0.03187 0.08298 -0.00309 -0.00441 0.00967 0.05969 0.00563 0.00016 0.00017 0.00031 0.00000 0.00185 0.00136 0.00229 0.00135 0.00142 0.00111 0.00083 C22 0.58634 0.42560 -0.02885 1.00000 0.05230 0.04590 0.08899 0.00237 0.00184 0.01497 0.06239 0.00925 0.00024 0.00029 0.00046 0.00000 0.00225 0.00220 0.00345 0.00217 0.00205 0.00179 0.00119 N23 0.59123 0.50467 0.00170 1.00000 0.05189 0.03787 0.13939 0.00389 0.00604 0.00975 0.07638 0.00906 0.00024 0.00025 0.00048 0.00000 0.00201 0.00182 0.00448 0.00217 0.00225 0.00157 0.00141 C24 0.58280 0.52804 0.11587 1.00000 0.09638 0.06312 0.13511 -0.02858 -0.03370 0.01685 0.09820 0.01103 0.00034 0.00036 0.00076 0.00000 0.00428 0.00327 0.00632 0.00381 0.00400 0.00291 0.00231 C25 0.60405 0.56312 -0.08400 1.00000 0.10101 0.07364 0.18164 0.04648 0.05280 0.02590 0.11876 0.01872 0.00042 0.00041 0.00085 0.00000 0.00465 0.00376 0.00836 0.00474 0.00539 0.00353 0.00303 O31 0.48764 0.25000 -0.08122 0.50000 0.05883 0.08743 0.08583 0.00000 -0.01996 0.00000 0.07737 0.00712 0.00026 0.00000 0.00050 0.00000 0.00261 0.00353 0.00368 0.00000 0.00257 0.00000 0.00142 C32 0.47999 0.25000 -0.17730 0.50000 0.10592 0.06365 0.10963 0.00000 -0.06842 0.00000 0.09307 0.01006 0.00052 0.00000 0.00086 0.00000 0.00620 0.00422 0.00669 0.00000 0.00568 0.00000 0.00304 N33 0.41922 0.25000 -0.23063 0.50000 0.11590 0.09838 0.16355 0.00000 -0.09559 0.00000 0.12594 0.01030 0.00051 0.00000 0.00100 0.00000 0.00712 0.00601 0.00957 0.00000 0.00715 0.00000 0.00415 C34 0.35375 0.25000 -0.16208 0.50000 0.08612 0.10326 0.42224 0.00000 -0.08377 0.00000 0.20387 0.02586 0.00069 0.00000 0.00227 0.00000 0.00807 0.00940 0.03863 0.00000 0.01348 0.00000 0.01244 C35 0.41535 0.25000 -0.34607 0.50000 0.18944 0.51176 0.19330 0.00000 -0.13154 0.00000 0.29817 0.02218 0.00124 0.00000 0.00209 0.00000 0.02113 0.04798 0.02302 0.00000 0.01926 0.00000 0.01665 O41 0.49725 0.25000 0.13717 0.50000 0.05557 0.09210 0.08499 0.00000 0.02511 0.00000 0.07755 0.00867 0.00026 0.00000 0.00050 0.00000 0.00255 0.00376 0.00365 0.00000 0.00242 0.00000 0.00146 C42 0.49615 0.25000 0.22936 0.50000 0.06591 0.12731 0.06729 0.00000 0.02323 0.00000 0.08684 0.01331 0.00043 0.00000 0.00073 0.00000 0.00436 0.00781 0.00457 0.00000 0.00361 0.00000 0.00258 N43 0.43395 0.25000 0.28405 0.50000 0.08077 0.21626 0.09638 0.00000 0.04243 0.00000 0.13113 0.01588 0.00047 0.00000 0.00085 0.00000 0.00530 0.01291 0.00641 0.00000 0.00462 0.00000 0.00424 C44 0.36853 0.25000 0.23625 0.50000 0.06421 0.08475 0.16020 0.00000 0.04371 0.00000 0.10305 0.01933 0.00047 0.00000 0.00116 0.00000 0.00471 0.00567 0.01069 0.00000 0.00555 0.00000 0.00358 C45 0.43494 0.25000 0.40555 0.50000 0.19871 1.08437 0.11902 0.00000 0.09292 0.00000 0.46737 0.04735 0.00154 0.00000 0.00201 0.00000 0.02346 0.11142 0.01630 0.00000 0.01686 0.00000 0.03543 O1 0.65456 0.25000 0.13528 0.50000 0.05100 0.02596 0.03931 0.00000 -0.00494 0.00000 0.03876 0.00462 0.00018 0.00000 0.00028 0.00000 0.00178 0.00133 0.00162 0.00000 0.00135 0.00000 0.00069 Final Structure Factor Calculation for NiClMelDMF Total number of l.s. parameters = 211 Maximum vector length = 623 Memory required = 41 / 2032 / 30527 wR2 = 0.2961 before cycle 21 for 5733 data and 0 / 211 parameters GooF = S = 1.118; Restrained GooF = 1.118 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1918 * P )^2 + 2.36 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 wR2 = 0.2961, GooF = S = 1.118, Restrained GooF = 1.118 for all data R1 = 0.0850 for 4374 Fo > 4sig(Fo) and 0.1043 for all 5733 data Occupancy sum of asymmetric unit = 21.00 for non-hydrogen and 0.00 for H and D atoms Principal mean square atomic displacements U 0.0414 0.0406 0.0298 Ni1 0.0637 0.0308 0.0305 Cl2 0.1000 0.0422 0.0367 Cl3 0.0530 0.0299 0.0258 N11 0.0473 0.0316 0.0260 C12 0.0947 0.0386 0.0265 N12 0.0631 0.0279 0.0233 N13 0.0544 0.0282 0.0240 C14 0.1122 0.0355 0.0232 N14 0.0622 0.0292 0.0233 N15 0.0475 0.0306 0.0248 C16 0.0783 0.0432 0.0233 N16 0.0845 0.0654 0.0291 O21 0.0893 0.0641 0.0338 C22 0.1400 0.0563 0.0329 N23 0.1654 0.0769 0.0524 C24 0.2263 0.0752 0.0548 C25 may be split into 0.6084 0.5670 -0.0706 and 0.5997 0.5592 -0.0974 0.0964 0.0874 0.0482 O31 0.1762 0.0637 0.0393 C32 0.2382 0.0984 0.0412 N33 0.4420 0.1033 0.0664 C34 may be split into 0.3502 0.2500 -0.1389 and 0.3573 0.2500 -0.1853 0.5118 0.3229 0.0598 C35 0.0994 0.0921 0.0412 O41 0.1273 0.0898 0.0434 C42 0.2163 0.1317 0.0454 N43 0.1771 0.0848 0.0473 C44 1.0844 0.2600 0.0578 C45 may be split into 0.4349 0.2775 0.4055 and 0.4349 0.2225 0.4055 0.0528 0.0375 0.0260 O1 ** Warning: 3 atoms may be split and 0 atoms NPD ** Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.005 0.009 0.015 0.020 0.026 0.033 0.044 0.062 0.097 1.000 Number in group 615. 541. 686. 526. 559. 511. 587. 564. 577. 567. GooF 1.152 1.269 1.196 1.012 1.007 0.890 1.194 1.096 0.982 1.269 K 3.161 1.445 1.205 1.076 1.017 0.996 1.063 1.029 1.046 0.987 Resolution(A) 0.71 0.74 0.77 0.80 0.84 0.90 0.97 1.07 1.22 1.54 inf Number in group 578. 576. 572. 578. 561. 576. 574. 575. 569. 574. GooF 0.837 0.793 0.759 0.778 0.760 0.813 0.831 0.976 1.080 2.435 K 0.996 1.029 1.022 1.011 1.022 1.021 1.024 1.009 1.032 0.986 R1 0.208 0.163 0.137 0.109 0.089 0.077 0.063 0.066 0.063 0.133 Recommended weighting scheme: WGHT 0.1927 2.2810 Most Disagreeable Reflections (* if suppressed or used for Rfree). Error/esd is calculated as sqrt(wD^2/) where w is given by the weight formula, D = Fo^2-Fc^2 and <> refers to the average over all reflections. h k l Fo^2 Fc^2 Error/esd Fc/Fc(max) Resolution(A) 3 2 1 4006.86 172.89 12.20 0.036 4.62 0 6 4 670.32 18.30 11.28 0.012 2.04 1 3 1 352.63 5.18 10.91 0.006 4.85 6 1 0 2245.93 299.38 9.36 0.047 3.08 1 2 1 8895.82 1407.56 8.41 0.101 6.43 0 2 2 1230.47 213.44 8.19 0.039 4.91 8 5 0 138.45 6.59 7.93 0.007 1.92 2 5 1 107.17 3.09 7.80 0.005 3.02 1 0 1 39.29 84737.59 7.12 0.786 10.25 2 0 0 -0.87 19769.30 7.11 0.380 9.41 2 4 2 1477.19 358.51 6.93 0.051 3.21 1 0 4 892.18 214.53 6.78 0.040 3.01 0 1 1 40.80 1704.84 6.69 0.112 9.82 3 3 4 238.38 44.21 6.59 0.018 2.46 4 0 0 18745.47 5198.58 6.45 0.195 4.71 3 0 1 701.61 11150.40 6.45 0.285 5.58 2 4 1 333.63 76.67 6.29 0.024 3.61 6 5 7 115.62 16.52 6.08 0.011 1.38 2 1 0 4029.56 33698.05 5.91 0.496 8.18 2 3 3 186.89 40.86 5.86 0.017 3.09 1 3 6 157.46 29.55 5.60 0.015 1.90 5 1 2 73.50 10.32 5.35 0.009 3.15 7 3 3 904.05 304.11 5.30 0.047 2.08 3 3 6 97.94 20.12 5.11 0.012 1.83 2 6 2 53.59 361.10 5.05 0.051 2.42 4 2 3 100.95 23.69 4.85 0.013 2.88 4 0 5 1929.37 736.03 4.84 0.073 2.17 4 4 4 359.14 122.58 4.84 0.030 2.18 1 9 11 60.17 0.41 4.76 0.002 0.95 2 6 0 1950.43 756.02 4.75 0.074 2.64 0 0 4 1330.69 5156.92 4.64 0.194 3.05 6 5 0 22.22 164.06 4.62 0.035 2.27 3 4 1 56.66 283.49 4.53 0.045 3.32 6 2 2 2796.16 1170.17 4.42 0.092 2.64 3 5 1 87.78 366.59 4.35 0.052 2.84 1 4 3 5956.48 2570.39 4.30 0.137 2.86 8 0 1 889.12 376.40 4.19 0.052 2.31 4 5 1 7.49 78.97 4.17 0.024 2.64 5 5 1 218.74 744.23 4.16 0.074 2.43 6 2 3 34.03 167.06 4.14 0.035 2.38 3 1 6 69.63 13.81 4.10 0.010 1.92 0 2 4 31.56 153.98 4.09 0.034 2.86 2 2 2 5878.59 2645.70 4.08 0.139 4.35 6 4 2 14.48 95.01 4.02 0.026 2.31 14 9 0 17.50 117.85 4.02 0.029 1.08 6 7 0 1313.30 586.62 3.99 0.065 1.88 11 2 7 28.48 0.52 3.95 0.002 1.21 1 1 1 2984.00 8646.03 3.95 0.251 8.71 6 6 5 24.78 1.97 3.89 0.004 1.58 4 2 6 42.02 8.35 3.84 0.008 1.82 Bond lengths and angles Ni1 - Distance Angles O21 2.0350 (0.0028) O21_$1 2.0350 (0.0028) 169.94 (0.22) O41 2.0476 (0.0048) 86.40 (0.10) 86.40 (0.10) O1 2.0544 (0.0033) 86.65 (0.10) 86.65 (0.10) 92.43 (0.21) O31 2.0587 (0.0049) 92.92 (0.09) 92.92 (0.09) 81.25 (0.25) 173.67 (0.20) Cl2 2.4184 (0.0013) 93.95 (0.10) 93.95 (0.10) 173.92 (0.18) 93.66 (0.11) 92.67 (0.17) Ni1 O21 O21_$1 O41 O1 O31 Cl2 - Distance Angles Ni1 2.4184 (0.0013) Cl2 N11 - Distance Angles C16 1.3402 (0.0037) C12 1.3534 (0.0037) 114.54 (0.25) N11 C16 C12 - Distance Angles N12 1.3338 (0.0039) N13 1.3472 (0.0038) 117.56 (0.27) N11 1.3534 (0.0037) 117.74 (0.28) 124.70 (0.27) C12 N12 N13 N12 - Distance Angles C12 1.3338 (0.0039) N12 N13 - Distance Angles C14 1.3370 (0.0037) C12 1.3472 (0.0038) 114.83 (0.25) N13 C14 C14 - Distance Angles N13 1.3370 (0.0037) N15 1.3480 (0.0035) 125.73 (0.26) N14 1.3491 (0.0038) 117.77 (0.26) 116.48 (0.27) C14 N13 N15 N14 - Distance Angles C14 1.3491 (0.0038) N14 N15 - Distance Angles C16 1.3381 (0.0039) C14 1.3480 (0.0035) 114.12 (0.25) N15 C16 C16 - Distance Angles N15 1.3381 (0.0039) N11 1.3402 (0.0037) 126.01 (0.26) N16 1.3571 (0.0037) 116.47 (0.27) 117.50 (0.28) C16 N15 N11 N16 - Distance Angles C16 1.3571 (0.0037) N16 O21 - Distance Angles C22 1.1862 (0.0058) Ni1 2.0350 (0.0028) 132.37 (0.35) O21 C22 C22 - Distance Angles O21 1.1862 (0.0058) N23 1.3604 (0.0064) 122.52 (0.52) C22 O21 N23 - Distance Angles C22 1.3604 (0.0064) C25 1.4437 (0.0086) 116.96 (0.61) C24 1.4555 (0.0099) 120.64 (0.51) 122.39 (0.55) N23 C22 C25 C24 - Distance Angles N23 1.4555 (0.0099) C24 C25 - Distance Angles N23 1.4437 (0.0086) C25 O31 - Distance Angles C32 1.1824 (0.0108) Ni1 2.0587 (0.0049) 133.91 (0.66) O31 C32 C32 - Distance Angles O31 1.1824 (0.0108) N33 1.3164 (0.0099) 126.65 (1.19) C32 O31 N33 - Distance Angles C32 1.3164 (0.0099) C35 1.4119 (0.0262) 122.61 (1.46) C34 1.4899 (0.0239) 116.15 (1.29) 121.24 (1.32) N33 C32 C35 C34 - Distance Angles N33 1.4899 (0.0239) C34 C35 - Distance Angles N33 1.4119 (0.0262) C35 O41 - Distance Angles C42 1.1262 (0.0097) Ni1 2.0476 (0.0048) 135.38 (0.58) O41 C42 C42 - Distance Angles O41 1.1262 (0.0097) N43 1.3480 (0.0102) 120.76 (0.94) C42 O41 N43 - Distance Angles C42 1.3480 (0.0102) C44 1.3628 (0.0155) 124.94 (1.10) C45 1.4841 (0.0265) 118.98 (1.40) 116.08 (1.36) N43 C42 C44 C44 - Distance Angles N43 1.3628 (0.0155) C44 C45 - Distance Angles N43 1.4841 (0.0265) C45 O1 - Distance Angles Ni1 2.0544 (0.0033) O1 FMAP and GRID set by program FMAP 2 2 22 GRID -1.316 -2 -1 1.316 2 1 R1 = 0.1023 for 5733 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 2.12 at 0.5044 0.0099 0.5212 [ 4.08 A from N15 ] Deepest hole -0.63 at 0.0675 0.0829 0.5014 [ 0.51 A from C22 ] Mean = 0.00, Rms deviation from mean = 0.24, Highest memory used = 2658 / 39531 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including eq.) Q1 1 0.9956 0.5099 0.0211 1.00000 0.05 2.12 4.08 N15 4.34 N15 4.41 C45 4.41 N14 Q2 1 0.9638 0.5628 0.1012 1.00000 0.05 1.72 3.25 N14 3.53 C14 3.59 N15 3.89 C35 Q3 1 0.4786 0.5748 0.3090 1.00000 0.05 1.53 3.16 C24 3.40 C32 3.41 N14 3.54 C35 Q4 1 0.5471 0.4734 0.4325 1.00000 0.05 1.35 3.52 N12 3.61 N15 4.03 C24 4.07 CL3 Q5 1 0.6808 0.2500 0.4712 0.50000 0.05 0.80 0.85 CL3 3.07 N12 3.10 N14 4.00 C34 Q6 1 0.8175 0.6527 0.1026 1.00000 0.05 0.65 0.87 N14 1.99 C14 2.49 CL3 2.51 N15 Q7 1 0.6991 0.3541 0.3382 1.00000 0.05 0.63 0.85 N12 1.92 C12 2.44 N11 2.60 CL3 Q8 1 0.4294 0.2500 -0.3668 0.50000 0.05 0.59 0.37 C35 1.67 N33 2.50 C32 2.78 C45 Q9 1 0.4326 0.1545 0.3617 1.00000 0.05 0.57 1.66 C45 1.84 N43 2.51 C44 2.55 C42 Q10 1 0.8074 0.6486 0.2180 1.00000 0.05 0.57 0.82 N14 1.89 C14 2.42 N13 2.57 CL2 Q11 1 0.3581 0.2261 -0.1994 1.00000 0.05 0.55 0.61 C34 1.28 N33 2.13 C35 2.34 C32 Q12 1 0.6170 0.2500 0.4992 0.50000 0.05 0.52 0.55 CL3 3.21 N14 3.61 C45 3.68 N12 Q13 1 0.7627 0.4202 -0.0937 1.00000 0.05 0.52 0.90 N16 1.94 C16 2.19 N13 2.42 N15 Q14 1 0.7369 0.3476 -0.0355 1.00000 0.05 0.49 0.84 N16 1.91 C16 2.43 N11 2.50 CL2 Q15 1 0.7129 0.4266 0.3993 1.00000 0.05 0.45 0.84 N12 1.93 C12 2.23 N15 2.47 N13 Q16 1 0.4208 0.2500 -0.4668 0.50000 0.05 0.44 1.48 C35 1.58 C45 2.88 N33 3.05 N43 Q17 1 0.4517 0.2062 0.2851 1.00000 0.05 0.43 0.80 N43 1.30 C42 1.67 C45 1.82 C44 Q18 1 0.3974 0.2500 -0.4195 0.50000 0.05 0.42 0.96 C35 2.25 C45 2.34 N33 3.25 C34 Q19 1 0.4541 0.2500 -0.4367 0.50000 0.05 0.40 1.33 C35 1.96 C45 2.60 N33 3.21 C32 Q20 1 0.3494 0.2500 0.2261 0.50000 0.05 0.40 0.38 C44 1.74 N43 2.72 C45 2.76 C42 Q21 1 0.5792 0.4261 0.0718 1.00000 0.05 0.39 0.99 O21 1.24 C22 1.57 N23 1.77 C24 Q22 1 0.3599 0.2101 -0.2911 1.00000 0.05 0.38 1.41 C35 1.49 N33 1.71 C34 2.73 C32 Q23 1 0.4669 0.2500 0.4737 0.50000 0.05 0.38 1.03 C45 2.40 N43 2.41 C35 3.03 C42 Q24 1 0.3886 0.2245 -0.4767 1.00000 0.05 0.37 1.73 C35 1.73 C45 3.07 N43 3.09 N33 Q25 1 0.4684 0.1650 -0.3600 1.00000 0.05 0.36 1.73 C35 2.31 N33 2.64 C32 3.25 C45 Q26 1 0.4902 0.2025 0.4205 1.00000 0.05 0.35 1.32 C45 2.12 N43 2.47 C42 2.91 CL3 Q27 1 0.3754 0.2500 -0.3450 0.50000 0.05 0.35 0.75 C35 1.62 N33 2.27 C34 2.84 C32 Q28 1 0.6199 0.2500 0.4217 0.50000 0.05 0.34 0.61 CL3 3.24 N12 3.31 C42 3.49 C45 Q29 1 0.4803 0.1968 -0.4037 1.00000 0.05 0.34 1.66 C35 2.56 N33 2.63 C45 2.90 C32 Q30 1 0.5272 0.1449 0.5205 1.00000 0.05 0.33 2.77 CL3 2.83 C45 3.18 C35 3.62 N14 Q31 1 0.5865 0.5682 0.1616 1.00000 0.05 0.33 0.87 C24 2.22 N23 3.02 C25 3.12 N33 Q32 1 0.6829 0.2073 0.1451 1.00000 0.05 0.33 0.89 O1 1.94 N11 2.64 NI1 2.78 O21 Q33 1 0.5787 0.5517 -0.1612 1.00000 0.05 0.32 1.07 C25 2.15 N23 2.64 C22 3.36 C24 Q34 1 0.3377 0.2500 0.4968 0.50000 0.05 0.32 2.14 C45 2.41 C35 2.79 N16 3.17 N43 Q35 1 0.6050 0.2500 0.4057 0.50000 0.05 0.30 0.93 CL3 2.97 C42 3.20 C45 3.35 N12 Q36 1 0.5291 0.2500 0.4202 0.50000 0.05 0.30 1.78 C45 2.08 CL3 2.41 C42 2.44 N43 Q37 1 0.2823 0.2500 -0.0159 0.50000 0.05 0.29 2.24 C34 2.82 CL3 3.16 N14 3.48 C44 Q38 1 0.4019 0.1544 -0.3796 1.00000 0.05 0.29 1.65 C35 2.43 N33 2.99 N16 3.12 C45 Q39 1 0.4192 0.1591 0.4564 1.00000 0.05 0.28 1.65 C45 2.60 N43 2.84 C35 3.22 C44 Q40 1 0.4397 0.1498 -0.3387 1.00000 0.05 0.28 1.72 C35 2.15 N33 2.68 C32 3.16 C34 Q41 1 0.3394 0.2010 0.2406 1.00000 0.05 0.28 0.98 C44 2.03 N43 2.81 N11 2.82 C45 Q42 1 0.3676 0.2500 0.1447 0.50000 0.05 0.27 1.12 C44 2.11 N43 2.44 O41 2.63 C42 Q43 1 0.5487 0.2179 0.4930 1.00000 0.05 0.25 1.76 CL3 2.45 C45 3.23 C35 3.39 N43 Q44 1 0.3822 0.2263 0.2992 1.00000 0.05 0.25 0.90 C44 1.07 N43 1.68 C45 2.34 C42 Q45 1 0.3910 0.2500 0.3149 0.50000 0.05 0.25 0.89 N43 1.05 C44 1.38 C45 2.24 C42 Q46 1 0.7371 0.4175 0.2046 1.00000 0.05 0.25 0.62 C12 0.74 N11 1.71 N12 1.77 N13 Q47 1 0.2584 0.2500 -0.0586 0.50000 0.05 0.24 2.19 C34 2.57 CL3 2.68 N14 3.63 C14 Q48 1 0.5683 0.2066 0.5247 1.00000 0.05 0.24 1.64 CL3 2.99 C45 3.21 N14 3.36 C35 Q49 1 0.3605 0.2500 -0.0786 0.50000 0.05 0.23 1.03 C34 2.16 N33 2.39 O31 2.55 C32 Q50 1 0.8389 0.6013 0.1549 1.00000 0.05 0.22 0.76 N14 1.41 C14 2.19 N15 2.39 N13 Q51 1 0.5661 0.6105 -0.0808 1.00000 0.05 0.22 1.06 C25 2.07 N23 2.68 O41 2.73 O21 Q52 1 0.3224 0.2500 0.0213 0.50000 0.05 0.21 2.32 C34 2.77 C44 3.35 O31 3.47 C25 Q53 1 0.3526 0.2500 0.3624 0.50000 0.05 0.21 1.57 C44 1.64 C45 1.81 N43 3.15 C42 Q54 1 0.3767 0.1989 -0.1239 1.00000 0.05 0.20 1.06 C34 1.75 N33 2.22 C32 2.31 O31 Q55 1 0.5027 0.2276 -0.1186 1.00000 0.05 0.20 0.65 O31 0.91 C32 2.12 N33 2.20 NI1 Q56 1 0.6142 0.5734 -0.0475 1.00000 0.05 0.20 0.51 C25 1.36 N23 2.21 C24 2.51 C22 Q57 1 0.6710 0.2099 0.5395 1.00000 0.05 0.19 1.31 CL3 2.08 N14 3.13 N14 3.18 C14 Q58 1 0.6535 0.6008 -0.0839 1.00000 0.05 0.19 1.12 C25 2.23 N23 2.70 N12 3.01 C12 Q59 1 0.3270 0.2056 0.0331 1.00000 0.05 0.19 2.54 C34 2.70 C44 2.76 C25 3.22 N12 Q60 1 0.3300 0.2228 0.4180 1.00000 0.05 0.18 2.03 C45 2.38 C44 2.59 N43 2.69 N16 Q61 1 0.3698 0.1551 -0.1962 1.00000 0.05 0.17 1.65 C34 1.87 N33 2.48 C24 2.56 C35 Q62 1 0.3369 0.1612 -0.0284 1.00000 0.05 0.17 2.22 C34 2.40 C25 2.87 C24 2.94 N23 Q63 1 0.3677 0.2018 -0.0452 1.00000 0.05 0.17 1.66 C34 2.43 O31 2.59 N33 2.77 C32 Q64 1 0.9004 0.6191 0.0462 1.00000 0.05 0.15 2.28 N14 2.48 CL3 2.89 C14 2.89 N15 Q65 1 0.3067 0.1880 0.1231 1.00000 0.05 0.15 2.08 C44 2.38 N12 2.70 C25 2.95 C12 Q66 1 0.3044 0.1915 -0.0159 1.00000 0.05 0.15 2.23 C34 2.91 N14 2.99 C25 3.19 N12 Q67 1 0.5323 0.4891 0.2630 1.00000 0.05 0.14 2.13 C24 3.39 N23 3.48 O21 3.48 C25 Q68 1 0.7398 0.1961 0.4452 1.00000 0.05 0.14 2.16 CL3 2.16 N12 2.99 N14 3.29 C12 Q69 1 0.6872 0.1864 0.4628 1.00000 0.05 0.14 1.43 CL3 2.18 N12 2.61 N14 3.21 N15 Q70 1 0.7507 0.4914 0.2473 1.00000 0.05 0.14 0.43 N13 0.92 C12 1.54 C14 1.96 N12 Q71 1 0.5912 0.4164 -0.1130 1.00000 0.05 0.14 1.04 C22 1.96 O21 2.02 N23 2.46 C25 Q72 1 0.7444 0.3398 0.4214 1.00000 0.05 0.14 1.58 N12 2.58 CL3 2.69 C12 3.04 N15 Q73 1 0.6652 0.1954 0.4020 1.00000 0.05 0.14 1.30 CL3 2.02 N12 3.20 C12 3.39 O1 Q74 1 0.7479 0.4087 0.1263 1.00000 0.05 0.14 0.48 N11 0.88 C16 1.56 C12 1.95 N15 Q75 1 0.7660 0.5263 0.2136 1.00000 0.05 0.13 0.53 N13 0.81 C14 1.61 C12 1.90 N14 Q76 1 0.8426 0.3677 0.1775 1.00000 0.05 0.13 2.08 N11 2.26 C44 2.37 C16 2.48 C12 Q77 1 0.7525 0.5389 0.2913 1.00000 0.05 0.13 0.61 N13 1.71 C14 1.77 C12 2.36 N14 Q78 1 0.8250 0.3437 -0.0821 1.00000 0.05 0.13 1.59 N16 2.46 C35 2.64 C16 3.28 N33 Q79 1 0.7473 0.1903 0.4926 1.00000 0.05 0.13 2.34 CL3 2.50 N14 2.53 N12 3.05 C34 Q80 1 0.7964 0.5001 0.0620 1.00000 0.05 0.13 0.34 N15 1.32 C16 1.45 C14 2.24 N16 Q81 1 0.8412 0.4329 0.2187 1.00000 0.05 0.13 2.02 C12 2.12 N13 2.24 N11 2.33 C14 Q82 1 0.7357 0.6579 0.1321 1.00000 0.05 0.12 1.44 N14 2.03 C14 2.30 C34 2.73 N15 Q83 1 0.3966 0.2500 -0.0381 0.50000 0.05 0.12 1.72 C34 1.79 O31 2.31 C32 2.39 N33 Q84 1 0.8643 0.4980 0.1636 1.00000 0.05 0.12 1.78 C14 2.03 N15 2.29 N13 2.38 N14 Q85 1 0.7873 0.3306 0.4230 1.00000 0.05 0.12 2.12 N12 2.70 C25 2.81 C44 2.96 C12 Q86 1 0.8308 0.4259 0.2461 1.00000 0.05 0.11 1.80 C12 2.02 N13 2.18 N11 2.42 C25 Q87 1 0.5607 0.4801 0.1705 1.00000 0.05 0.11 1.12 C24 2.18 N23 2.44 O21 2.64 C22 Q88 1 0.5294 0.2122 0.2409 1.00000 0.05 0.11 0.89 C42 1.54 O41 1.97 N43 2.76 C45 Q89 1 0.7802 0.5267 0.1013 1.00000 0.05 0.11 0.57 N15 0.78 C14 1.66 C16 1.82 N14 Q90 1 0.7600 0.4166 0.0996 1.00000 0.05 0.11 0.51 C16 0.89 N11 1.65 N16 1.66 N15 Q91 1 0.5269 0.2500 0.3105 0.50000 0.05 0.11 1.15 C42 1.78 N43 2.08 C45 2.19 O41 Q92 1 0.7684 0.5119 0.2825 1.00000 0.05 0.10 0.41 N13 1.43 C12 1.64 C14 2.18 N12 Q93 1 0.7692 0.3420 0.3613 1.00000 0.05 0.10 1.50 N12 2.22 C12 2.69 C44 2.75 N11 Q94 1 0.7342 0.6407 0.0757 1.00000 0.05 0.10 1.69 N14 2.03 C14 2.33 N15 2.67 C34 Q95 1 0.4510 0.2500 -0.2097 0.50000 0.05 0.10 0.65 N33 0.67 C32 1.71 O31 1.80 C35 Q96 1 0.5354 0.2500 -0.2446 0.50000 0.05 0.09 1.33 C32 2.19 O31 2.19 N33 2.58 C35 Q97 1 0.4270 0.1581 -0.1963 1.00000 0.05 0.09 1.58 N33 1.83 C32 2.09 C34 2.36 O31 Q98 1 0.5201 0.2500 -0.3299 0.50000 0.05 0.09 1.98 C35 2.01 C32 2.25 N33 3.10 O31 Q99 1 0.5707 0.3701 -0.0265 1.00000 0.05 0.08 0.75 O21 0.96 C22 2.06 NI1 2.28 N23 Q100 1 0.4346 0.2500 -0.0999 0.50000 0.05 0.08 1.02 O31 1.27 C32 1.62 N33 1.70 C34 Shortest distances between peaks (including symmetry equivalents) 28 35 0.34 81 86 0.40 74 90 0.42 44 45 0.47 77 92 0.55 43 48 0.57 68 79 0.60 1 1 0.63 70 92 0.64 25 40 0.65 68 72 0.67 37 47 0.69 80 89 0.72 16 18 0.73 16 19 0.73 16 18 0.73 16 19 0.73 55 55 0.74 65 85 0.74 82 94 0.74 16 24 0.75 52 59 0.75 70 75 0.76 59 66 0.77 25 29 0.78 44 44 0.78 11 11 0.79 62 66 0.80 72 85 0.82 18 24 0.83 49 83 0.84 24 24 0.84 85 93 0.85 20 41 0.85 69 73 0.86 72 93 0.87 38 40 0.87 75 92 0.87 8 18 0.88 37 52 0.88 65 93 0.88 60 60 0.90 49 63 0.90 62 63 0.91 53 60 0.92 45 53 0.93 12 28 0.95 70 77 0.95 63 83 0.97 8 19 0.97 56 58 0.97 22 27 0.98 54 63 0.98 46 74 0.99 18 27 1.00 72 79 1.00 75 77 1.00 68 69 1.03 44 53 1.03 68 85 1.03 83 100 1.04 8 27 1.05 37 66 1.05 20 42 1.05 49 54 1.05 88 91 1.06 43 43 1.06 57 69 1.06 5 69 1.06 59 62 1.07 34 60 1.07 26 36 1.07 61 97 1.08 5 57 1.08 96 98 1.08 19 29 1.08 11 54 1.08 18 19 1.09 24 34 1.09 59 85 1.10 36 43 1.10 23 26 1.11 66 79 1.11 52 66 1.12 19 23 1.12 16 23 1.13 6 50 1.14 54 61 1.15 2 3 1.15 11 22 1.15 20 44 1.15 41 44 1.16 12 35 1.16 51 56 1.17 9 39 1.18 79 85 1.19 76 81 1.19 69 79 1.19 11 61 1.19 59 65 1.20 12 48 1.20 37 79 1.22 59 63 1.23 8 16 1.23 66 85 1.24 6 57 1.24 10 50 1.25 5 12 1.25 88 88 1.25 63 66 1.26 67 87 1.26 28 73 1.26 69 72 1.27 37 59 1.27 5 73 1.27 1 4 1.27 30 48 1.28 25 38 1.29 47 79 1.29 76 86 1.29 5 28 1.30 7 73 1.30 12 57 1.31 30 43 1.31 9 17 1.32 22 22 1.32 68 93 1.32 57 57 1.32 66 94 1.33 20 45 1.34 23 36 1.34 36 91 1.34 81 84 1.34 7 72 1.35 29 40 1.35 79 94 1.35 46 70 1.35 46 90 1.35 55 100 1.35 43 48 1.36 71 99 1.36 17 44 1.36 7 93 1.36 65 72 1.37 8 29 1.38 1 4 1.38 95 100 1.38 12 43 1.39 19 24 1.39 54 83 1.40 47 66 1.40 75 89 1.40 17 45 1.40 33 51 1.40 54 100 1.41 32 32 1.41 49 52 1.42 49 100 1.42 52 63 1.42 6 10 1.42 7 15 1.43 48 48 1.43 26 43 1.44 35 36 1.44 1 2 1.44 17 17 1.45 35 73 1.45 5 68 1.46 54 97 1.46 30 64 1.46 29 98 1.46 59 59 1.47 24 39 1.47 37 68 1.47 13 14 1.48 22 61 1.48 66 68 1.49 62 94 1.50 68 73 1.50 41 76 1.51 65 68 1.52 18 34 1.52 54 62 1.52 41 42 1.52 9 26 1.52 38 78 1.52 55 95 1.52 21 99 1.52 11 49 1.53 31 87 1.54 11 22 1.54 21 87 1.54 29 30 1.54 47 52 1.55 59 79 1.55 41 45 1.56 42 65 1.56 17 88 1.56 31 97 1.56 26 26 1.57 52 83 1.57 15 72 1.57 41 65 1.58 26 39 1.58 57 79 1.58 48 64 1.58 33 56 1.58 11 54 1.58 13 77 1.58 6 82 1.58 8 25 1.58 58 85 1.59 63 63 1.59 95 97 1.59 35 43 1.59 62 85 1.60 8 24 1.60 80 90 1.60 52 62 1.61 41 44 1.61 6 94 1.61 5 79 1.61 72 73 1.62 16 29 1.62 41 41 1.62 17 91 1.62 49 66 1.62 22 38 1.62 16 34 1.63 63 100 1.63 52 85 1.63 5 35 1.64 52 65 1.64 36 48 1.64 23 43 1.64 95 96 1.64 49 62 1.65 23 24 1.65 18 38 1.65 51 58 1.65 2 64 1.66 29 38 1.66 37 49 1.66 20 53 1.66 34 53 1.67 8 38 1.67 59 68 1.67 49 59 1.67 24 38 1.68 7 69 1.68 24 27 1.68 47 68 1.68 84 86 1.68 28 43 1.68 2 30 1.68 54 54 1.69 58 65 1.69 24 60 1.69 66 72 1.70 26 30 1.70 9 44 1.70 55 96 1.70 57 73 1.70 65 66 1.70 66 82 1.70 8 40 1.70 26 91 1.70 58 62 1.71 31 61 1.71 19 25 1.71 27 38 1.71 28 36 1.71 41 53 1.71 16 27 1.72 11 97 1.72 10 82 1.72 28 69 1.72 42 59 1.72 17 44 1.73 7 68 1.73 13 78 1.73 42 52 1.73 8 22 1.73 52 79 1.73 59 83 1.73 79 93 1.74 28 48 1.74 44 76 1.74 12 73 1.74 12 69 1.74 25 98 1.75 57 68 1.75 37 85 1.75 44 60 1.75 23 29 1.75 14 78 1.75 29 29 1.76 40 97 1.76 23 39 1.76 35 48 1.76 45 60 1.76 8 98 1.77 47 82 1.77 16 39 1.77 50 84 1.77 68 68 1.78 50 89 1.78 80 84 1.78 50 64 1.79 47 57 1.79 6 64 1.79 24 78 1.79 37 62 1.80 6 69 1.80 9 76 1.80 11 95 1.80 18 29 1.80 19 98 1.80 65 79 1.80 73 73 1.80 62 79 1.81 17 26 1.81 20 65 1.81 5 47 1.81 59 72 1.81 15 93 1.81 79 82 1.81 84 89 1.82 47 94 1.82 3 67 1.83 37 63 1.83 52 68 1.84 29 43 1.84 46 86 1.84 18 22 1.84 18 23 1.85 9 45 1.85 11 27 1.85 59 66 1.85 62 83 1.85 28 57 1.85 70 86 1.86 19 27 1.86 89 90 1.86 58 93 1.86 47 59 1.86 59 93 1.86 25 30 1.86 62 82 1.86 58 59 1.87 35 91 1.87 33 58 1.88 46 75 1.88 34 78 1.88 29 48 1.88 22 40 1.89 86 92 1.90 3 25 1.90 54 66 1.90 22 78 1.90 68 94 1.90 73 79 1.90 24 60 1.91 54 63 1.91 60 76 1.91 12 36 1.92 22 97 1.92 6 79 1.92 46 92 1.92 11 100 1.93 97 100 1.93 26 43 1.93 66 66 1.93 74 80 1.93 11 63 1.93 16 38 1.94 47 49 1.94 54 95 1.94 48 57 1.94 44 60 1.94 26 48 1.95 42 44 1.95 41 93 1.95 56 62 1.95 72 94 1.95 70 89 1.96 59 63 1.96 95 98 1.96 8 95 1.96 69 85 1.97 85 94 1.97 68 79 1.97 37 94 1.97 13 92 1.97 79 79 1.97 11 61 1.97 57 69 1.98 46 81 1.98 50 75 1.98 19 38 1.98 62 65 1.99 75 80 1.99 5 37 1.99 70 81 1.99 76 90 1.99 7 85 1.99 24 29 2.00 35 69 2.00 61 63 2.00 5 72 2.00 43 64 2.00 66 83 2.00 75 84 2.00 3 40 2.01 74 76 2.01 37 72 2.01 53 76 2.01 70 74 2.01 57 64 2.01 27 78 2.02 19 26 2.03 38 39 2.03 69 93 2.03 37 65 2.03 39 60 2.04 81 92 2.05 65 65 2.05 19 43 2.05 27 40 2.05 14 90 2.05 16 26 2.05 27 34 2.06 19 40 2.06 59 94 2.06 17 88 2.06 18 78 2.06 55 97 2.06 1 2 2.06 74 89 2.06 7 46 2.07 47 69 2.07 18 25 2.07 31 67 2.07 8 23 2.07 22 54 2.08 66 93 2.08 15 69 2.08 33 86 2.08 18 40 2.08 58 66 2.09 22 95 2.09 89 94 2.09 75 81 2.09 19 39 2.09 75 86 2.10 69 69 2.10 4 67 2.11 41 86 2.11 59 65 2.11 37 82 2.11 73 93 2.11 47 62 2.11 16 25 2.11 33 81 2.12 48 98 2.12 24 53 2.12 30 36 2.12 42 45 2.12 74 81 2.13 81 90 2.13 69 73 2.13 23 48 2.13 49 61 2.13 15 85 2.13 61 82 2.13 11 83 2.14 54 59 2.14 58 86 2.14 61 62 2.14 45 76 2.15 25 97 2.15 23 30 2.15 29 39 2.15 2 4 2.15 26 29 2.16 63 66 2.16 35 57 2.16 58 72 2.16 74 86 2.16 69 94 2.16 57 72 2.16 15 68 2.16 57 94 2.16 10 75 2.16 24 39 2.17 37 83 2.17 62 68 2.17 2 25 2.17 18 39 2.17 50 80 2.17 50 82 2.17 46 76 2.17 37 69 2.17 42 85 2.18 62 72 2.18 17 20 2.18 9 53 2.18 27 95 2.18 40 61 2.18 9 23 2.18 17 41 2.18 68 69 2.19 30 39 2.19 2 4 2.19 70 90 2.19 7 65 2.19 47 85 2.19 63 85 2.19 6 89 2.19 61 95 2.19 76 84 2.19 52 72 2.20 63 94 2.20 34 39 2.20 41 60 2.20 15 73 2.21 47 63 2.21 17 53 2.21 52 54 2.21 28 91 2.21 6 47 2.22 7 79 2.22 37 57 2.22 10 94 2.22 54 82 2.22 39 76 2.22 14 74 2.23 64 69 2.23 11 63 2.24 86 90 2.24 89 92 2.24 74 75 2.24 40 98 2.24 66 79 2.25 19 36 2.25 11 82 2.25 25 27 2.25 47 72 2.25 55 83 2.26 15 70 2.26 12 64 2.26 57 82 2.26 59 85 2.26 4 30 2.26 16 60 2.26 15 92 2.26 57 79 2.26 41 81 2.26 39 53 2.27 1 30 2.27 10 77 2.27 5 6 2.27 21 71 2.27 63 97 2.27 19 30 2.27 20 76 2.28 27 29 2.28 36 88 2.28 32 74 2.28 46 77 2.28 41 85 2.29 75 90 2.29 29 43 2.29 60 78 2.29 2 84 2.29 4 64 2.29 50 57 2.29 38 97 2.29 50 94 2.29 86 93 2.29 23 91 2.29 43 98 2.29 24 25 2.29 40 95 2.29 57 73 2.30 42 83 2.30 24 40 2.30 66 69 2.30 59 79 2.30 16 40 2.30 26 35 2.31 61 100 2.31 11 97 2.31 31 54 2.31 17 39 2.31 9 44 2.31 19 48 2.31 52 93 2.32 24 26 2.32 17 36 2.32 6 68 2.32 26 88 2.32 38 61 2.32 33 71 2.32 59 68 2.32 39 44 2.32 30 43 2.32 57 68 2.33 5 48 2.33 43 91 2.33 84 92 2.33 58 63 2.33 59 62 2.33 22 25 2.33 15 79 2.33 63 82 2.33 15 80 2.33 25 95 2.33 83 95 2.33 68 73 2.34 19 34 2.34 24 29 2.34 Time profile in seconds ----------------------- 0.00: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.00: Generate connectivity array 0.00: Analyse DFIX and DANG restraints 0.00: Analyse SAME, SADI and NCSY restraints 0.00: Generate CHIV restraints 0.00: Check if bonds in residues restrained 0.00: Generate DELU and RIGU restraints 0.00: Generate SIMU restraints 0.00: Generate ISOR restraints 0.00: Analyse electron density 0.00: Analyse other restraints etc. 0.03: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.03: Set up l.s. refinement 0.00: Generate idealized H-atoms 0.28: Structure factors and derivatives 0.25: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 0.03: Solve l.s. equations 0.00: Generate HTAB table 0.09: Other dependent quantities, CIF, tables 0.03: Analysis of variance 0.05: Merge reflections for Fourier and .fcf 0.02: Fourier summations 0.00: Peaksearch 0.00: Analyse peaklist ** WARNING: These times are only approximate for multiple threads. To get better estimates run with -t1 ** Please cite: G.M. Sheldrick (2015) "Crystal structure refinement with SHELXL", Acta Cryst., C71, 3-8 (Open Access) if SHELXL proves useful. +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + shelx finished at 17:27:10 Total elapsed time: 0.81 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++