Single step site-selective reaction to construct a Ag2Au2 ← Ag4 supramolecular assembly from hybrid N-heterocyclic carbene (NHC): synthesis, structures and optoelectronic properties
Das, Pooja; Halder, Soumi; Ray, Partha Pratim; Jana, Narayan Ch.; Sahu, Priyanka; Isab, Anvarhusein A.; Dandela, Rambabu; Natarajan, Ramalingam; Dinda, Joydev; RSC Advances 15 (2025) 13086–13094; doi:10.1039/D5RA00684H

data_7250319
_publ_section_title
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 Single step site-selective reaction to construct a Ag2Au2 \\leftarrow Ag4
 supramolecular assembly from hybrid N-heterocyclic carbene (NHC):
 synthesis, structures and optoelectronic properties
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_journal_issue                   17
_journal_name_full               'RSC Advances'
_journal_page_first              13086
_journal_page_last               13094
_journal_paper_doi               10.1039/D5RA00684H
_journal_volume                  15
_journal_year                    2025
_chemical_formula_moiety         'C26 H22 Ag Au N6, 2(F6 P), 2(C2 H3 N)'
_chemical_formula_sum            'C30 H28 Ag Au F12 N8 P2'
_chemical_formula_weight         1095.38
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2025-03-10
_audit_creation_method
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Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
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2025-03-12 deposited with the CCDC.	2025-04-09 downloaded from the CCDC.
;
_cell_angle_alpha                68.601(2)
_cell_angle_beta                 82.896(2)
_cell_angle_gamma                66.589(2)
_cell_formula_units_Z            2
_cell_length_a                   12.2152(9)
_cell_length_b                   12.9415(10)
_cell_length_c                   13.7513(11)
_cell_measurement_reflns_used    9973
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      0.755
_cell_measurement_theta_min      0.725
_cell_volume                     1856.8(3)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2016/6 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      273.15
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0670
_diffrn_reflns_av_unetI/netI     0.0565
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            35469
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.552
_diffrn_reflns_theta_min         2.386
_exptl_absorpt_coefficient_mu    4.655
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.4846
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1021 before and 0.0737 after correction.
The Ratio of minimum to maximum transmission is 0.6499.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'light white'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    1.959
_exptl_crystal_description       block
_exptl_crystal_F_000             1056
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.236
_refine_diff_density_min         -0.998
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     615
_refine_ls_number_reflns         8503
_refine_ls_number_restraints     189
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0523
_refine_ls_R_factor_gt           0.0356
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0212P)^2^+1.8011P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0743
_refine_ls_wR_factor_ref         0.0830
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6902
_reflns_number_total             8503
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ra00684h2.cif
_cod_data_source_block           au_3p1_pf6_0m_a
_cod_database_code               7250319
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.653
_shelx_estimated_absorpt_t_min   0.456
_olex2_refinement_description
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1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H28A,H28B,H28C} of C28, All C(H,H) groups
 At 1.5 times of:
  {H30A,H30B,H30C} of C30
2. Restrained distances
 F9-F13 \\sim F10-F16 \\sim F15-F14 \\sim F11-F17 \\sim F7-F8 \\sim F18-F12
 with sigma of 0.04
3. Rigid body (RIGU) restrains
 F13, F9, F10, F16, F11, F17, F8, F7, F15, F14, F12, F18, P6B
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 F5B, F5A, F4A, F4B, F3B, F3A, F2A, F2B, F1A, F1B, F6B, F6A, P1B, P1A
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 P6B, P6A
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
4. Others
 Fixed Sof: P1B(0.5) F3B(0.5) F2B(0.5) F1B(0.5) F5B(0.5) F4B(0.5) F6B(0.5)
 P6B(0.5) F15(0.5) F12(0.5) F7(0.5) F13(0.5) F17(0.5) F16(0.5) F10(0.5)
 F18(0.5) F11(0.5) F8(0.5) F9(0.5) F14(0.5) F5A(0.5) F4A(0.5) P1A(0.5) F3A(0.5)
 F2A(0.5) F1A(0.5) F6A(0.5) P6A(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C21(H21A,H21B), C8(H8A,H8B)
5.b Aromatic/amide H refined with riding coordinates:
 C15(H15), C26(H26), C2(H2), C16(H16), C7(H7), C20(H20), C13(H13), C23(H23),
 C10(H10), C3(H3), C18(H18), C25(H25), C12(H12), C17(H17), C24(H24), C11(H11),
 C5(H5), C4(H4)
5.c Idealised Me refined as rotating group:
 C28(H28A,H28B,H28C), C30(H30A,H30B,H30C)
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_shelx_res_checksum              63048
_olex2_submission_special_instructions 'No special instructions were received'