Electrocatalytic nitrogen reduction to ammonia by graphene-supported Au<sub>4</sub>Cu<sub>2</sub> and Au<sub>2</sub>Ag<sub>2</sub> nanoclusters.
Shehzad, Aamir; Yi, Qiuhao; Cui, Chaonan; Luo, Zhixun; Nanoscale 17 (2025) 7453–7459; doi:10.1039/d4nr05341a

data_1573943
_publ_section_title
;
 Electrocatalytic nitrogen reduction to ammonia by graphene-supported
 Au<sub>4</sub>Cu<sub>2</sub> and Au<sub>2</sub>Ag<sub>2</sub>
 nanoclusters.
;
_journal_issue                   12
_journal_name_full               Nanoscale
_journal_page_first              7453
_journal_page_last               7459
_journal_paper_doi               10.1039/d4nr05341a
_journal_volume                  17
_journal_year                    2025
_chemical_formula_moiety         'C68 H50 Ag2 Au2 P2'
_chemical_formula_sum            'C68 H50 Ag2 Au2 P2'
_chemical_formula_weight         1538.69
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-11-30
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_audit_update_record
;
2024-01-20 deposited with the CCDC.	2025-02-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.7590(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.3993(2)
_cell_length_b                   21.6280(3)
_cell_length_c                   21.9620(3)
_cell_measurement_reflns_used    28208
_cell_measurement_temperature    110.01(10)
_cell_measurement_theta_max      31.2490
_cell_measurement_theta_min      1.9160
_cell_volume                     5402.95(14)
_computing_cell_refinement       'CrysAlisPro 1.171.39.45i (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.45i (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.45i (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      110.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.855
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w      0.00  52.00   0.50    3.00    --  -11.60  45.00 156.38  104
  2  \w   -101.00  -9.00   0.50    3.00    --  -11.60  45.00  90.00  184
  3  \w     13.00  76.00   0.50    3.00    --  -11.60  45.00  90.00  126
  4  \w   -101.00 -18.00   0.50    3.00    --  -11.60  45.00 156.38  166
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC10 (RCD3): fixed-chi single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0418638000
_diffrn_orient_matrix_UB_12      0.0016983000
_diffrn_orient_matrix_UB_13      -0.0224552000
_diffrn_orient_matrix_UB_21      0.0154331000
_diffrn_orient_matrix_UB_22      0.0303411000
_diffrn_orient_matrix_UB_23      0.0099132000
_diffrn_orient_matrix_UB_31      0.0436240000
_diffrn_orient_matrix_UB_32      -0.0123340000
_diffrn_orient_matrix_UB_33      0.0210603000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0235
_diffrn_reflns_av_unetI/netI     0.0271
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.855
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            45818
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.855
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.021
_diffrn_reflns_theta_min         1.883
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    6.230
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63790
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.45i (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.892
_exptl_crystal_description       block
_exptl_crystal_F_000             2960
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.331
_refine_diff_density_min         -1.841
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     667
_refine_ls_number_reflns         14759
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0310
_refine_ls_R_factor_gt           0.0259
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0232P)^2^+15.8653P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0598
_refine_ls_wR_factor_ref         0.0612
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13293
_reflns_number_total             14759
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4nr05341a2.cif
_cod_data_source_block           mx8936
_cod_depositor_comments
'Adding full bibliography for 1573943--1573945.cif.'
_cod_database_code               1573943
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         AuAgCH
_reflns_odcompleteness_completeness 99.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C12(H12), C13(H13), C14(H14),
 C15(H15), C16(H16), C18(H18), C19(H19), C20(H20), C21(H21), C22(H22), C24(H24),
  C25(H25), C26(H26), C27(H27), C28(H28), C30(H30), C31(H31), C32(H32),
 C33(H33), C34(H34), C38(H38), C39(H39), C40(H40), C41(H41), C42(H42), C46(H46),
  C47(H47), C48(H48), C49(H49), C50(H50), C52(H52), C53(H53), C54(H54),
 C55(H55), C56(H56), C58(H58), C59(H59), C60(H60), C61(H61), C62(H62), C64(H64),
  C65(H65), C66(H66), C67(H67), C68(H68)
;
_shelx_res_checksum              13501
_shelx_hkl_checksum              74592
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.313
_oxdiff_exptl_absorpt_empirical_full_min 0.693