Supplementary material Studies on preparation and hydrogen storage properties of dual-metal ferrocenyl coordination polymer microspheres Ruoli Sun, Li Wang*, Haojie Yu*, Zain-ul-Abdin, Yongsheng Chen, Hamad Khalid, Nasir Abbasi, Muhammad Akram, Sergey Z. Vatsadze, Dmitri A. Lemenovskii Experimental High pressure H2 storage measurements: All measurements were made with ultrahigh purity grade (99.999%) H2. Approximately 0.2 g of the sample was placed in the steel cell and degassed at 373 K for a minimum of 6 h under vacuum. When H2 was passed through, the hydrogen pressure in 2 (Scheme 1) was increased and recorded step by step from vacuum to about 4 MPa at 163 K, with a balance time of 5 min at each step. Then needle valve 12 was opened and pressure was balanced for 5 min. The value of the system pressure was recorded on a M400 software. For comparison, a blank measurement was conducted at 163 K to get basic data before measurements of the samples. The final hydrogen storage capacity was obtained by subtracting the result from sample with that from blank without sample measured at the same conditions. Scheme 1. Schematic representation of Sievert’s apparatus for hydrogen adsorption.[11b] 1,Ultra-high-purity hydrogen; 2, buffer tube; 3, pressure meter; 4, pressure sensor; 5, computer; 6, ultra-low/constant-temperature stirring reaction bath; 7, sample cell; 8, vacuum pump; 9, volume- measurement equipment by drainage method; 10-15, needle valves, 16 and 17, air release valves. 1 Figure S1. Laser particle analyze of dual metal coordination polymers microspheres (dispersion liquid: ethanol). Figure S2. SEM images of single metal coordination polymers, (A and B: Co-CPs, C and D: Mn-CPs, E and F: Cu-CPs. Reaction condition: metal:ligand=1:1, 150 oC, 12 h). 2 Figure S3. TEM images of dual metal coordination polymer microspheres after hydrogen storage. (A: CoMn-1, B:CoMn-2, C:CoCu-1, D: CoCu-2, E: MnCu-1, F: MnCu-2) 3