Synthesis of a Labile Sulfur-Centred Ligand, [S(H)C(PPh 2 S) 2 ] : Structural Diversity in Lithium(I), Zinc(II) and Nickel(II) Complexes
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1 Electronic Supplementary Material (ESI) for Dalton Transactions. This journal is The Royal Society of Chemistry 2016 Electronic Supplementary Information (ESI): Synthesis of a Labile Sulfur-Centred Ligand, [S(H)C(PPh 2 S) 2 ] : Structural Diversity in Lithium(I), Zinc(II) and Nickel(II) Complexes Ramalingam Thirumoorthi, a Tristram Chivers, a Susanna Häggman, b Akseli Mansikkamäki, b Ian S. Morgan, b Heikki M. Tuononen, b Manu Lahtinen b and Jari Konu*,b a Department of Chemistry, University of Calgary, Calgary, AB T2N 1N4, Canada. b Department of Chemistry, University of Jyväskylä, P.O. Box 35, Jyväskylä, FI-40014, Finland. X-ray powder diffraction data 2 UV-Vis spectroscopic data 4 Additional computational data 5 Optimized Cartesian coordinates 6 1
2 X-ray powder diffraction data (XRPD): Experimental The bulk powder sample of {Ni[S(H)C(PPh 2 S) 2 ] 2 }(5b) was examined by X-ray powder diffraction (XRPD) using a PANalytical X Pert PRO diffractometer at room temperature. Primary beam Johansson monochromator was used to produce CuK α1 radiation ( Å; 45kV, 40mA). Each sample was prepared on to a siliconmade sample holder (producing zero-background signal) using petrolatum jelly as an adhesive. Diffraction pattern was collected with a position sensitive X Celerator detector in a continuous scanning mode using 2θ-range of 3-70 with a step size of and recording time of 40 s per step. HighScore Plus (v. 4.1) 1 program was used to examine the data and the DASH program 2 for the auto-indexing (with sub-program DICVOL) 3 and whole-pattern Pawley refinement of the patterns. Results Truncated 2θ-range of 5-50 with first 25 diffraction peak positions were used as an input for the autoindexing procedure in order to search the best fitting unit cell parameters. As the result all the peaks were indexed by triclinic unit cell settings a = (38) Å, b = (38) Å, c = (29) Å, α = (25) β= (24), γ = (22) and V = Å 3 with reasonable figure of merits (M 25 = 36.7, F 25 = (0.0060, 31). 4 Prior to Pawley refinement P-1 space group was assigned based on the settings determined by single crystal analysis, and the unit cell settings afforded by the indexing were converted to correspond settings of the single crystal structure. Extraction of individual diffraction intensities by Pawley refinement process lead to good agreement between observed and calculated pattern with χ 2 = 1.40 (413 reflections; R wp = % and R exp = %) with refined unit cell setting shown in the Table S1. Table S1. Crystallographic parameters of 5b and its bulk powder. Parameters single crystal powder a (Å) (5) b (Å) (5) c (Å) (5) α ( ) (5) β ( ) (5) γ ( ) (5) V (Å 3 ) T ( o C)
3 Figure S1. Whole-pattern Pawley refinement plot, Bragg peak positions are indicated by the bars on top. Experimental pattern is shown in red, calculated in blue and residual in light purple colour. References: 1. HighScore plus 4.1, PANalytical BV. Almelo, Netherlands, W. I. F. Shankland, J. van de Streek, E. Pidcock, W. D. S. Motherwell and J. C. Cole, J. Appl. Cryst., 2006, 39, A. Boultif, and D. Louër, Powder pattern indexing with the dichotomy method, J. Appl. Cryst., 2004, 37, P. M. De Wolff, A simplified criterion for the reliability of a powder pattern indexing, J. Appl. Crystallogr., 1968, 1,
4 UV-Vis spectroscopic data: Figure S2. Comparison of the measured (5b) and calculated (5a, 5b, 5b and 5c) UV-Vis spectra. Figure S3. UV-Vis spectra of the square-planar Ni(II) isomer 5b measured at (a) 23 o C, and (b) -50 o C. 4
5 Table S2. Calculated TDDFT excitation wavelengths and oscillator strengths greater than a 5b 5b' 5c λ [nm] f osc λ [nm] f osc λ [nm] f osc λ [nm] f osc Additional computational data: Table S3. Absolute energies, enthalpies and Gibbs' free energies of optimized structures at 298 K (in Hartree atomic units). E H G 5a b b' c
6 Optimized Cartesian coordinates: 5a Ni P P S S S C C H C H C H C H C H C C H C H C H C H C H C C H C H C H C H C H C C H C H C H C H C H C H P P S S S C C H C H C H C H C H C C H C H C H C H C H C C H C H C H C H C H C C H C H C H C H C H C H b' Ni P P S S S C C H C H C H C H C H C C H C H C H C H C H C C H C H C H
7 C H C H C C H C H C H C H C H C H P P S S S C C H C H C H C H C H C C H C H C H C H C H C C H C H C H C H C H C C H C H C H C H C H C H c Ni S S S P P C C H C H C H C H C H C C H C H C H C H C H C C H C H C H C H C H C C H C H C H C H C H C H S S S P P C C H C H C H C H C H C C H C H C H C H
8 C H C C H C H C H C H C H C C H C H C H C H C
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