Supplementary Figure 1 IR Spectroscopy. 1Cu 1Ni Supplementary Figure 2 UV/Vis Spectroscopy. 1Cu 1Ni
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1 Supplementary Figure 1 IR Spectroscopy. IR spectra of 1Cu and 1Ni as well as of the starting compounds, recorded as KBr-pellets on a Bruker Alpha FTIR spectrometer. Supplementary Figure 2 UV/Vis Spectroscopy. UV/Vis spectra of 1Cu and 1Ni recorded in acetonitrile solution at room temperature on a Perkin-Elmer Lambda 2 spectrometer. 1
2 Supplementary Figure 3 Susceptibility temperature product as a function of temperature for 1Cu. The measurement was performed on a teflon-wrapped pressed powder sample in an applied field of 1000 Oe with a Quantum Design MPMS XL7 SQUID magnetometer. The data were corrected for the diamagnetic contribution by using Pascal's constants. 1,0 Brillouin functions 1.8 K 2 K 3 K 5 K 7 K 10 K M / B 0,5 0, H / koe Supplementary Figure 4 Magnetization as a function of field for 1Cu. The measurement was performed on a teflon-wrapped pressed powder sample at various temperatures as indicated in the Figure with a Quantum Design MPMS XL7 SQUID magnetometer. The data were corrected for the diamagnetic contribution by using Pascal's constants. Solid red lines are fits to the Brillouin function with S = ½ and g =
3 a b Intensity (arb. u.) Intensity (arb. u.) Magnetic field (mt) Supplementary Figure 5 CW X-band EPR spectra of 1Cu 1.5%. Experimental CW X-Band EPR spectra (blue solid lines) and easy spin simulations (red dashed lines). The spectra were recorded on a finely ground powder sample of 1Cu 1.5% in evacuated sample tubes at 9.47 GHz on a Bruker EMX spectrometer in Stuttgart. a, Spectrum at 5 K and fit with parameters g = ± 0.002, g = ± 0.001, A = 496 ± 5 MHz, A = 119 ± 5 MHz. b, Spectrum at room temperature and fit with parameters g = ± 0.002, g = ± 0.001, A = 480 ± 5 MHz, A = 115 ± 5 MHz. 3
4 a b c d Intensity (arb. u.) e f Magnetic field (mt) Magnetic field (mt) Supplementary Figure 6 Pulsed Q-band EPR spectra of 1Cu 0.001%. Electron spin echo detected field-swept spectra recorded on 1Cu 0.001% (blue solid lines) and easy spin simulations (red dashed lines) using the parameters g = ± 0.010, g = ± 0.005, A = 500 ± 5 MHz, A = 118 ± 5 MHz. The measurements were performed on a Bruker Elexsys E580 in Frankfurt. Temperatures up to 275 K were achieved with an Oxford Instruments CF935 continuous flow cryostat (cryogenic liquid: He), room temperature measurements were done at approximately 294 K. a, Spectrum recorded at 7 K and GHz. b, Spectrum recorded at 15 K and GHz. c, Spectrum recorded at 50 K and 33.8 GHz. d, Spectrum recorded at 120 K and GHz. e, Spectrum recorded at 200 K and GHz. f, Spectrum recorded at room temperature and GHz. 4
5 Supplementary Figure 7 Hahn echo decay curves of 1Cu 0.001%. Normalized echo intensity as a function of delay time 2τ (Hahn echo sequence) recorded on a powder sample of 1Cu 0.001% at different temperatures. Black solid lines are stretched exponential fits resulting in the coherence times reported in Supplementary Table 1. The measurements were performed at 34 GHz on a Bruker Elexsys E580 in Frankfurt. Temperatures up to 275 K were achieved with an Oxford Instruments CF935 continuous flow cryostat (cryogenic liquid: He), room temperature measurements were done at approximately 294 K. 5
6 Intensity / arb. u. 0,3 0,2 0,1 0,0 1,16 1,20 1,24 1,28 Magnetic Field / T a / arb. units I*I 1 0 I / arb. units 1,0 0,8 0,6 0,4 0,2 0, b / s 15 c T / ms Supplementary Figure 8 Pulsed EPR on 1Cu 1.5%. The measurements were performed at 35 GHz on a homebuilt pulsed Q-band EPR spectrometer in Stuttgart. a, echo detected EPR spectrum recorded at 7 K; b, Hahn echo decay curve at 7 K together with stretched exponential fit, where T M = 3.97 μs, and x = 1.43; c, inversion recovery curve together with a biexponential fit at 7 K, where T 1,f = 2.5 ms and T 1,s = 41 ms. 6
7 Supplementary Figure 9 Nutation measurement of 1Cu 0.001%. Nutation measurement on a powder sample of 1Cu 0.001% at 15 K and different applied powers were performed at 34 GHz on a Bruker Elexsys E580 in Frankfurt. Pulse sequence: nutation pulse - τ nut - π/2 - τ fix - π - τ fix - echo with τ nut = 400 ns, τ fix = 140 ns. 7
8 Supplementary Figure 10 Inversion recovery traces of 1Cu 0.001%. Normalized echo intensity as a function of delay time T (inversion recovery sequence) at different temperatures. Black solid lines are biexponential (for 7-25 K) or monoexponential (for T > 25 K) fit functions resulting in the spin lattice relaxation times reported in Supplementary Table 2. The measurements were performed at 34 GHz on a Bruker Elexsys E580 in Frankfurt. Temperatures up to 275 K were achieved with an Oxford Instruments CF935 continuous flow cryostat (cryogenic liquid: He), room temperature measurements were done at approximately 294 K. 8
9 Intensity / arb. u. 0,05 0,04 0,03 0,02 0,01 0,00 1,16 1,20 1,24 1,28 Magnetic Field / mt a Echo Intensity / arb. u. 1,0 7 K b 50 K 150 K 0, / s 1,5 1,0 0,5 0,0-0,5-1, T / s c Supplementary Figure 11 Pulsed EPR on 1Cu 0.01% D. The measurements were performed at 35 GHz on a homebuilt pulsed Q-band EPR spectrometer in Stuttgart. a, echo detected EPR spectrum recorded at 7 K; b, Hahn echo decay curves together with fit functions at different temperatures; c, inversion recovery curves together with fit functions at different temperatures. Fit functions are bi- (7 K) or monoexponentials (50, 100 K) for both relaxation times and their results are reported in Supplementary Table 3. 9
10 Supplementary Table 1 Coherence times T M and stretch factors for 1Cu 0.001%. Parameters were extracted from fitting Hahn echo decay curves of Supplementary Figure 7 with stretched exponentials. T / K T M / μs x ± ± ± ± ± ± ± ± ± ± ± ± ± ± ± ± ± ± ± ± ± ± ± ± ± ± ± ± ± ± ± ± ± ± ± ± ± ± rt ± ± Supplementary Table 2 Spin lattice relaxation times T 1 (fast and slow components) for Cu 0.001%. Parameters were extracted from fitting Inversion recovery traces of Supplementary Figure 10 with biexponential (for 7-25 K) or monoexponential (for T > 25 K) fit functions. T / K T 1,f / μs T 1,s / μs rt
11 Supplementary Table 3 Spin lattice relaxation times T 1 and spin-spin relaxation times T M (fast and slow components in both cases) for Cu 0.01% D. Parameters were extracted from fitting Inversion recovery traces and Hahn echo decays shown in Supplementary Figure 11 with biexponential (for 7 K) or monoexponential (for 50, 100 K) fit functions. T / K T 1,f / μs T 1,s / μs T M,f / μs T M,s / μs 7 7 ± ± ± ± ± ± ± ± 0.2 Supplemetary Methods Synthesis and Analysis All reagents and solvents were used as purchased from commercial sources. Bis-(tetraphenylphosphonium)-bis-(maleonitriledithiolato)cuprate, (PPh 4 ) 2 [Cu(mnt) 2 ] (1Cu): Sodium maleonitriledithiolate (279 mg, 1.5 mmol) was dissolved in 5 ml ethanol and 2 ml demineralized water. Subsequently copper chloride dihydrate (128 mg, 0.75 mmol), dissolved in 5 ml ethanol, and tetraphenylphosphonium bromide (629 mg, 1.50 mmol), dissolved in 15 ml ethanol were added under stirring. The brown product precipitated immediately and was separated from the solution after 5 min by vacuum filtration. Washing of the product with 3 x 5 ml ethanol and drying for 20 h under reduced pressure gave a yield of 576 mg (75.01 % based on Cu). Elemental analysis: found (calcd) for C 59 H 40 CuN 4 P 2 S 4 in %: C: (65.77), H: 3.90 (3.94), N: 5.48 (5.48), S: (12.54). UV/VIS (MeCN): λ max in nm: 478, 430, 369, 348, 317, 275. IR (KBr-pellet): in cm -1 and assignment in brackets: 2195 (ν C N ), 1459 (ν C=C ). Bis-(tetraphenylphosphonium)-bis-(maleonitriledithiolato)nickelate (PPh 4 ) 2 [Ni(mnt) 2 ] (1Ni): The same procedure as described for 1Cu was executed with nickel chloride hexahydrate (178 mg, 0.75 mmol) instead of copper chloride dihydrate. The red compound was isolated with a yield of 614 mg (80.4 % based on Ni). Elemental analysis: found (calcd) for C 59 H 40 NiN 4 P 2 S 4 : C: (66.08), H: 3.94 (3.96), N: 5.46 (5.50), S: (12.60). UV/VIS (MeCN): λ max in nm: 474, 379, 315, 270. IR (KBr-pellet): in cm -1 and assignment in brackets: 2196 (ν C N ), 1479 (ν C=C ). Perdeuterotetraphenylphosphonium bromide PPh 4 Br -d 20 : In a pressure cylinder, deuterated triphenylphosphine ( g, 3.6 mmol) was combined with anhydrous nickel(ii)bromide ( g, 1.8 mmol) and deuterated phenylbromide (0.76 ml, 7.2 mmol). The pressure cylinder was sealed and heated to 180 C for three hours. After cooling, 50 ml of demineralized water was added to the blue-green solid. After stirring for 15 min at 75 C, a watery blue solution and a fawn precipitate formed. The mixture was cooled in an ice bath and extracted with 3 x 50 ml of diethylether. The organic phase of the ether extraction was discarded and the aqueous phase was extracted with 3 x 50 ml chloroform. Subsequently, the solvent of the organic phase was removed and the resulting white solid was dried under reduced pressure. 13 C NMR (500MHz): (t), (td), (td), , ppm. 11
12 Bis-(perdeuterotetraphenylphosphonium)-bis-(maleonitriledithiolato)cuprate (PPh 4 -d 20 ) 2 [Cu(mnt) 2 ] (1CuD): The deuterated compound was synthesized following the same procedure as described for its protonated analogue, except that PPh 4 Br was replaced by d 20 -PPh 4 Br. UV/VIS in DCM: λ max in nm: 482, 388, 373, 328, 323, 287, 276, 268. IR (KBrpellet): in cm -1 and assignment in brackets: 2195 (ν C N ), 1459 (ν C=C ). Bis-(perdeuterotetraphenylphosphonium)-bis-(maleonitriledithiolato)nickelate (PPh 4 -d 20 ) 2 [Ni(mnt) 2 ] (1NiD): The deuterated complex was synthesized following the same procedure as given for its protonated analogue above, where PPh 4 Br was replaced by d 20 - PPh 4 Br. UV/VIS in DCM: λ max in nm: 481, 384, 318, 272, 229. IR (KBr-pellet): in cm -1 and assignment in brackets: 2195 (ν C N ), 1479 (ν C=C ). Doped powder: % of 1Cu in 1Ni (1Cu 0.001% ): Doped powders 1Cu 0.001% were obtained by dissolving compounds 1Cu and 1Ni in the molar ratio : in a minimum volume of acetone, which was subsequently evaporated under reduced pressure. The resulting powders were dried in vacuo and finely ground. Doped powder: 0.01 % of 1CuD in 1NiD (1Cu 0.01% D): Doped powders 1Cu 0.01% D wereobtained similarly to 1Cu 0.001% from 1CuD and 1NiD. Doped single crystal: 1.5 % of 1Cu in 1Ni (1Cu 1.5% ): X-ray quality single crystals were obtained by dissolving compounds 1Cu and 1Ni in the molar ratio 98.5 : 1.5 in a minimum volume of acetone, which was subsequently diluted with the same amount of methanol. Crystals were collected after one week of slow solvent evaporation under ambient conditions. Results of X-ray analysis of 1Cu 1.5% : monoclinic, a = (10), b = (13), c = (12) Å, β = (5), V = (4) Å 3, T = 110 K, space group P2 1 /n, Z = 4, reflections collected, 7183 unique, final R 1 = , wr 2 [I > 2σ(I)] = , GOF =
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