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RESEARCH PAPER · Angewandte Chemie International Edition · 2022

Doping‐Mediated Energy‐Level Engineering of M@Au 12 Superatoms (M=Pd, Pt, Rh, Ir) for Efficient Photoluminescence and Photocatalysis

Haru Hirai, Shinjiro Takano, Takuya Nakashima, Takeshi Iwasa, Tetsuya Taketsugu, Tatsuya Tsukuda

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Doping‐Mediated Energy‐Level Engineering of M@Au 12 Superatoms (M=Pd, Pt, Rh, Ir) for Efficient Photoluminescence and PhotocatalysisOriginalTargeted Synthesis of Ligand-Protected Gold Clusters and Exploration of Their Design Principles0Theoretical and experimental study of organometallic transition metal nanoclusters and nanoparticles0Depletion Driven Assembly of Ultrasmall Metal Nanoclusters: From Kinetically Arrested Assemblies to Thermodynamically Stable, Spherical Superclusters19Near-Infrared Dual Emission from the Au 42 (SR) 32 Nanocluster and Tailoring of Intersystem Crossing117Supervalence Bonding in Bi-icosahedral Cores of [M1Au37(SC2H4Ph)24]− (M = Pd and Pt): Fusion-Mediated Synthesis and Anion Photoelectron Spectroscopy27Effects of Single Platinum Atom Doping on Stability and Nonlinear Optical Properties of Ag29 Nanoclusters25Alloying and dealloying of Au 18 Cu 32 nanoclusters at precise locations via controlling the electronegativity of substituent groups on thiol ligands12IrAu 12 superatom modified by chiral diphosphines: doping-induced enhancement of chiroptical activity22Spontaneous Intercluster Electron Transfer X 2– + X 0 → 2 X – (X = PtAu 24 (SC n H 2 n +1 ) 18 ) in Solution: Promotion by Long Alkyl Chains18Electronegativity of the Substituent on Surface Motifs Influences the Ultrafast Relaxation Dynamics of Ag44(SR)304– Nanoclusters16Atom‐Precise Heteroatom Core‐Tailoring of Nanoclusters for Enhanced Solar Hydrogen Generation75Effect of Group-10 Element M (Ni, Pd, Pt) on Electronic Structure of Icosahedral M@Au 12 Cores of MAu 24 L 18 (L = Alkynyl, Thiolate)12Atomically Precise Metal Nanoclusters as Single Electron Transferers for Hydroborylation33Structurally Flexible Au–Cu Alloy Nanoclusters Enabling Efficient Triplet Sensitization and Photon Upconversion73Bimetallic Sites for Catalysis: From Binuclear Metal Sites to Bimetallic Nanoclusters and Nanoparticles689Internal quantum efficiency higher than 100% achieved by combining doping and quantum effects for photocatalytic overall water splitting298Excited State Engineering in Ag29 Nanocluster through Peripheral Modification with Silver(I) Complexes for Bright Near-Infrared Photoluminescence57Superatom‐in‐Superatom Nanoclusters: Synthesis, Structure, and Photoluminescence30Superatom‐in‐Superatom Nanoclusters: Synthesis, Structure, and Photoluminescence5Preorganized Nitrogen Sites for Au 11 Amidation: A Generalizable Strategy toward Precision Functionalization of Metal Nanoclusters76A compressed structure construction and transformation in metal nanoclusters4Luminescence modulation of ultrasmall gold clusters by aromatic ligands24Effect of Silver Alloying on the Vibrational Dynamics of Rod-Shaped Gold Nanoclusters13Hydride Doping Effects on the Structure and Properties of Eight-Electron Rh/Ag Superatoms: The [RhH x @Ag 21– x {S 2 P(O n Pr) 2 } 12 ] ( x = 0–2) Series40Isostructural Nanocluster Manipulation Reveals Pivotal Role of One Surface Atom in Click Chemistry88Isostructural Nanocluster Manipulation Reveals Pivotal Role of One Surface Atom in Click Chemistry8Dual Catalysis of Gold Nanoclusters:Photocatalytic Cross-Dehydrogenative Coupling by Cooperation of Superatomic Core and Molecularly Modified Staples0In Situ Depletion-Guided Engineering of Nanoshell-like Gold Nanocluster Assemblies with Enhanced Peroxidase-like Nanozyme Activity21Elucidating the Near-Infrared Photoluminescence Mechanism of Homometal and Doped M25(SR)18 Nanoclusters134Visible to NIR‐II Photoluminescence of Atomically Precise Gold Nanoclusters189Dual Catalysis of Gold Nanoclusters: Photocatalytic Cross‐Dehydrogenative Coupling by Cooperation of Superatomic Core and Molecularly Modified Staples**6Dual Catalysis of Gold Nanoclusters: Photocatalytic Cross‐Dehydrogenative Coupling by Cooperation of Superatomic Core and Molecularly Modified Staples**43Single thiolate replacement of metal nanoclusters10Tailoring Carbon Tails of Ligands on Au 52 (SR) 32 Nanoclusters Enhances the Near-Infrared Photoluminescence Quantum Yield from 3.8 to 18.3%133Dissecting the Triplet-State Properties and Intersystem Crossing Mechanism of the Ligand-Protected Au13 Superatom34Exciton and vibrational dynamics of MAu24(SR)18 (M=Pd, Pt) nanoclusters3Constructing perfect cubic Ag–Cu alloyed nanoclusters through selective elimination of phosphine ligands3Bonding and Electronic Interactions of Hydrogen with Gold Superatoms18Effect of Specific Heavy Doping of Silver Atoms into the Icosahedral Au 13 on Electronic Structure and Catalytic Performance13“Sergeants-and-soldiers” principle in the synthesis of intrinsically chiral Au 13 clusters3Assembly of anionic silver nanoclusters with controlled packing structures through site-specific ionic bridges4Atomically precise Au and Ag nanoclusters doped with a single atom as model alloy catalysts50Bright near-infrared emission from the Au 39 (SR) 29 nanocluster30Circular dichroism and circularly polarized luminescence of ligand-protected molecular metal clusters: insights into structure–chiroptical property relationships20Doping-mediated excited state dynamics of diphosphine-protected M@Au 12 (M = Au, Ir) superatom nanoclusters11Oxygen insertion at the cage center: an unconventional tuning strategy for enhancing the photocatalytic performance of atomically precise copper cluster cocatalysts5Revisiting ultrasmall phosphine-stabilized rhodium-doped gold clusters Au n Rh ( n = 5, 6, 7, 8): geometric, electronic, and vibrational properties3Synthesis of atomically precise Ag 16 nanoclusters and investigating solvent-dependent ultrafast relaxation dynamics4Synthesis of RhH-doped Au–Ag alloy nanoclusters and dopant evolution3Tailoring two magic number Au 13 nanoclusters with N-containing diphosphine ligands: a classical icosahedral core vs. an unprecedented UFO- shaped core6Triplet properties and intersystem crossing mechanism of PtAg28 nanocluster sensitizers achieving low threshold and efficient photon upconversion22Triplet–triplet annihilation-based photon upconversion using nanoparticles and nanoclusters36Tuning photoluminescence properties of Au clusters by surface modification and doping: lessons from case studies of icosahedral Au 1325Introducing Iodide Ligands on IrAu 12 Cluster Enhances Phosphorescence Efficiency and Photoredox Activity11Diphosphine‐Protected IrAu12 Superatom with Open Site(s): Synthesis and Programmed Stepwise Assembly0Diphosphine‐Protected IrAu12 Superatom with Open Site(s): Synthesis and Programmed Stepwise Assembly31Unraveling a Concerted Proton-Coupled Electron Transfer Pathway in Atomically Precise Gold Nanoclusters48Photoluminescent Characterization of Metal Nanoclusters: Basic Parameters, Methods, and Applications128Au36(SR)22 Nanocluster and a Periodic Pattern from Six to Fourteen Free Electrons in Core Size Evolution15CPL in Chiral Metal Nanoclusters0Nanocluster Chemistry and the Role of in Situ Fluorescence as an Analytical Tool9NIR-II emissive anionic copper nanoclusters with intrinsic photoredox activity in single-electron transfer51RhRu Bimetallic Oxide Cluster Catalysts for Cross-Dehydrogenative Coupling of Arenes and Carboxylic Acids9Synthesis of N2-Type Superatomic Molecules26Unraveling the Solvent Regulation in the Heteroatom-Doped Endohedral Gold Clusters: A Theoretical Study on the Electronic Properties and O2 Activation2Golden insights from a silver superatom2Isomeric Effects of Au28(S-c-C6H11)20 Nanoclusters on Photoluminescence: Roles of Electron-Vibration Coupling and Higher Triplet State46If the Crown Fits: Sterically Demanding N-Heterocyclic Carbene Promotes the Formation of Au8Pt Nanoclusters6Molecular Interactions in Atomically Precise Metal Nanoclusters46Impact of the Peripheral Ligand Layer on the Excited-State Deactivation Mechanism of Au38S2(S-Adm)20 and Au30(S-Adm)18 (S-Adm = Adamantanethiolate) Clusters13Loading Lewis Acid/Base Pair on Metal Nanocluster for Catalytic Ugi Reaction4Loading Lewis Acid/Base Pair on Metal Nanocluster for Catalytic Ugi Reaction39Raising Near-Infrared Photoluminescence Quantum Yield of Au 42 Quantum Rod to 50% in Solutions and 75% in Films24Au25 Cluster-Based Atomically Precise Coordination Frameworks and Emission Engineering through Lattice Symmetry19Substrate-Dependent Role of a Pd Dopant in PdAu12 Catalysts in the Oxidation of p-Substituted Benzyl Alcohols: Promotion of Hydride Abstraction and Reductive Activation of O217Photosynthesis of Au8Cu6 nanocluster for photocatalysis in oxidative functionalization of alkynes32In situ QXAFS study of CO and H 2 adsorption on Pt in [PtAu 8 (PPh 3 ) 8 ]-H[PMo 12 O 40 ] solid3Harnessing NIR-II luminescence in ultrasmall gold nanoparticles for enhanced biomedical applications7Chemical Synthesis of ~1 nm Multilevel Capacitor‐like Particles with Atomic Precision7Chemical Synthesis of ~1 nm Multilevel Capacitor‐like Particles with Atomic Precision3Heterogeneous Catalysis of Molecular‐Like Au8M(PPh3)8n+ Clusters Cultivated in Mesoporous SBA‐1513Heterogeneous Catalysis of Molecular‐Like Au8M(PPh3)8n+ Clusters Cultivated in Mesoporous SBA‐150Recent Advances in Understanding Triplet States in Metal Nanoclusters: Their Formation, Energy Transfer, and Applications in Photon Upconversion34Intramolecular Aggregation‐Induced Surface Coupling of Metal Nanoclusters: Structure Elucidation and Photoluminescence Manipulation16A comprehensive review of atomically precise metal nanoclusters with emergent photophysical properties towards diverse applications171Pd Nanoparticles Decorated by Oxidized Ru Clusters for Efficient C–H/C–H Coupling of Arenes4A nearly perfect icosahedral Ir@Au 12 superatom with superior photoluminescence obtained by ligand engineering14An icosahedral Au 13 nanocluster with three adjacent chlorides on opposite poles catalyses hydroamination of phenylacetylene1An Rh–Au nanocluster protected by an N-heterocyclic carbene: synthesis, structure, and single-molecule conductance properties0Atom-precise coinage metal nanoclusters for near-infrared emission: excited-state dynamics and mechanisms59Intensive near-infrared emitting Au 7 Cu 10 nanoclusters for both energy and electron harvesting17Sequential adsorption of multiple CO molecules on Au 10 − and Au 9 Zn − triangular clusters: the crucial role of a single atomic impurity0Summary and Prospects0Surface ligand networking promotes intersystem crossing in the Au 18 (SR) 14 nanocluster8Synthesis planning for atomically precise metal nanoclusters8近红外二区金团簇在生物荧光成像中的应用（特邀）1Unlocking the Photoluminescence and Photostability of Au11 Clusters through Pt‐Mediated Band‐Gap Engineering1Unraveling the Stoichiometric Interactions and Synergism between Ligand-Protected Gold Nanoparticles and Proteins34Superatomic catalyst for efficient nitric oxide reduction using Al8O3 superatom-oxide framework2Site-specific substitution in atomically precise carboranethiol-protected nanoclusters and concomitant changes in electronic properties41Metal Nanoclusters as Highly Efficient, Versatile Type‐II Photoinitiators via Generating Radicals from Non‐Conventional Hydrogen Donors8Metal Nanoclusters as Highly Efficient, Versatile Type‐II Photoinitiators via Generating Radicals from Non‐Conventional Hydrogen Donors0Atomically Engineered Trimetallic Nanoclusters Toward Enhanced Photoluminescence and Photoinitiation Activity22Preparation Methods of Metal Nanoclusters6Halide‐Directed Ligand Engineering Enables Expedient, Controlled and Divergent Syntheses of Diphosphine‐Protected Au Nanoclusters14Shell engineering of an atomically precise PdH-doped Cu nanocluster0Enhancement of Photoluminescence Quantum Yield of Silver Clusters by Heavy Atom Effect18Precise Composition Control of Supported Au Cluster Catalyst for Evaluating Catalytic Properties0Electrochemical Carbon Dioxide Reduction Reaction or Hydrogen Evolution Reaction: Kernel and Type‐Dependent Catalytic Activity of Staples in Metal Nanoclusters7Poisoning Electrocatalytic CO2 Conversion to CO by Adding a μ4-S Atom on Au60 Nanocluster5Unprecedented stacking-dependent piezoluminescence enhancement in atomically precise superatomic gold nanoclusters11Evolution of coherent vibrations in atomically precise gold quantum rods with periodic elongation18Gram-Scale Synthesis of a Laccase-Like Cu 36 Nanocluster with Enhanced Catalytic Activity and Stability25Heterometal Doping Modulates Luminescent and Chiroptical Behavior in Superatomic M₁Ag₁₄ (M = Pd, Pt) Clusters7Atomically Precise Alloy Nanoclusters Steering Photocatalysis74Pressure-Activated Efficient Near-Infrared Luminescence in Atomically Precise Gold Nanoclusters20Johnson Solid Gold Nanoclusters as Heterogeneous Visible-Light Photocatalysts for Fukuyama Indole Synthesis29Single‐Site Metal‐Nonmetal Microenvironment Regulation of Copper Nanoclusters with Atomic Precision for X‐Ray Imaging18Single‐Site Metal‐Nonmetal Microenvironment Regulation of Copper Nanoclusters with Atomic Precision for X‐Ray Imaging1High-Yield Synthesis of Cu29 Nanoclusters and Their Applications in Photothermal Conversion and Catalysis12Visualization of Total Synthesis from Au 11 to Au 13 Nanoclusters16Functionalization of Gold-Pincer Nanocluster for Asymmetric Catalysis29Selective heterometal doping in isostructural clusters converts phosphorescence to TADF with over 100-fold enhancing5X-ray Crystallographic Visualization of a Nucleation and Anisotropic Growth in Thiolate-Protected Gold Clusters: Toward Targeted Synthesis of Gold Quantum Needles33Structural Flexibility-Driven Dual Emission Switching in Ultrathin Gold Nanorod Clusters16Insights into the excited-state behavior of metal nanoclusters: from structure-based properties to dynamic control via ionic association10Understanding the NIR Emission of Metal Nanoclusters Through a Ligand-Shell-Kernel Triad Picture12Emerging Opportunities of Metal Nanoclusters for Photocatalytic Organic Synthesis15Understanding Excited States in Magic Series Au 8 n +4 (SR) 4 n +8 Nanoclusters: Role of Size, Ligands, and Theory Level7Fully Reversible Photoelectronic Switching Enabled by Delocalized Excitons in a Single Superatom Junction7Stepwise Ligand-Exchange Strategy for the High-Yield Synthesis of Water-Soluble, Metal-Doped MAg 24 Nanoclusters3Atomically Precise Coinage Metal Nanocluster Photocatalysts: Recent Advances in Organic Synthesis16Nanoclusters as Deep‐Red Light‐Absorbing Photocatalysts for Laser‐ or LED‐Driven Povarov Cyclization10Manipulating the Intersystem Crossing Process in Atomically Precise Gold Nanoclusters7Photoluminescence and Excited-State Dynamics of Gold–Copper Nanoclusters6Highly efficient near-infrared phosphorescence from aggregated gold nanoclusters with humidity response0Atomically precise nanoclusters of coinage metals for photothermal energy conversion: recent progress and biomedical applications0Computational exploration of N-heterocyclic carbene (NHC)-for-phenylacetylene ligand exchange in IrAu 12 alloy clusters1Introducing chiral ligands with rigidity into the achiral Au 21 cluster for constructing CPL nanomaterials0Photoluminescence of ligand-protected gold nanoclusters: progress in experimental and theoretical studies5Atomically Precise Metal Nanoclusters for Near-Infrared-II Photonics22Multifaceted Molecular Design Enables Comprehensive Luminescence Modulation in Metalloligand‐Stabilized Gold Nanoclusters6Au 42 (PET) 32 Nanocluster Sensitizer Unlocks the Annihilator Potential of Rubrene, Enabling High‐Performance NIR‐to‐Visible Photon Upconversion6Ligand Modulation Triggers Metal Nanocluster NIR-II Photocatalysis3Microsecond-Lived Luminescence in Semiconductor Quantum Dots and Metal Nanoclusters: Unveiling a Common Origin0Orthogonal Quintuple‐Stimuli Responsiveness in an Ultrastable, Ultrabright Cu 16 Nanocluster via Molecular and Supramolecular Engineering0High‐Throughput Screening and Interpretable Machine Learning for Rational Design of Bimetallic Catalysts for Methane Activation2Gold Quantum Rods Emit in the Shortwave Infrared (1000–2200 nm) with 10 4–5 M –1 cm –1 Ultrabrightness15Ultrafast Intersystem Crossing in Icosahedral-Core Metal Nanoclusters4One Atom Makes a Big Difference in NHC‐Ligated Alloy Nanoclusters: From Structure and Properties to Catalysis6

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  10. Electronegativity of the Substituent on Surface Motifs Influences the Ultrafast Relaxation Dynamics of Ag44(SR)304– Nanoclusters

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  12. Effect of Group-10 Element M (Ni, Pd, Pt) on Electronic Structure of Icosahedral M@Au 12 Cores of MAu 24 L 18 (L = Alkynyl, Thiolate)

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  40. “Sergeants-and-soldiers” principle in the synthesis of intrinsically chiral Au 13 clusters

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