1：Experimental Design and Method Selection:

Hydrothermal synthesis was used to construct the MOFs, with variations in solvents, pH, and auxiliary ligands to achieve different structures. Characterization methods included IR spectroscopy, PXRD, TGA, single-crystal X-ray diffraction, luminescence measurements, and gas adsorption experiments.

2：Sample Selection and Data Sources:

Samples were synthesized from commercially available reagents including H5L ligand, Cd(NO3)2·4H2O, and bib ligand. Data were collected from synthesized crystals and their suspensions in aqueous solutions for sensing studies.

3：List of Experimental Equipment and Materials:

Equipment included Vario MACRO analyzer for elemental analysis, FTIR-8400s spectrometer for IR, Rigaku D/Max-2500 PC diffractometer for PXRD, METTLER TGA analyzer for thermal analysis, F-4600 fluorescence spectrophotometer for luminescence, ASAP-2020 analyzer for gas adsorption, and Bruker Apex II CCD diffractometer for single-crystal X-ray diffraction. Materials included ethanol, water, NaOH, and various ions in nitrate or salt forms.

4：Experimental Procedures and Operational Workflow:

Synthesis involved dissolving reagents in solvent mixtures, adjusting pH, heating in sealed tubes, and cooling to obtain crystals. Characterization steps included IR, PXRD, TGA, luminescence titrations with ion additions, and gas adsorption isotherm measurements at different temperatures.

5：Data Analysis Methods:

Structural data were solved using OLEX-2 and refined with SHELXL-2015; topological analyses used TOPOS4.0. Luminescence data were analyzed using Stern-Volmer equations to calculate quenching constants and detection limits. Gas adsorption data were used to calculate surface areas and uptake amounts.