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_7250318
_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 Ag2 N6, 2(F6 P), 2(C2 H3 N)'
_chemical_formula_sum            'C30 H28 Ag2 F12 N8 P2'
_chemical_formula_weight         1006.28
_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             2025-03-03
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-03-12 deposited with the CCDC.	2025-04-09 downloaded from the CCDC.
;
_cell_angle_alpha                68.2040(10)
_cell_angle_beta                 82.8810(10)
_cell_angle_gamma                66.6170(10)
_cell_formula_units_Z            2
_cell_length_a                   12.1446(5)
_cell_length_b                   12.9632(5)
_cell_length_c                   13.8516(6)
_cell_measurement_reflns_used    5830
_cell_measurement_temperature    273.15
_cell_measurement_theta_max      25.26
_cell_measurement_theta_min      2.98
_cell_volume                     1857.81(13)
_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 0.987
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type
'SuperNova, Dual, Cu at home/near, Pilatus 200K'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0452
_diffrn_reflns_av_unetI/netI     0.0388
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            35032
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.511
_diffrn_reflns_theta_min         2.386
_exptl_absorpt_coefficient_mu    1.236
_exptl_absorpt_correction_T_max  0.885
_exptl_absorpt_correction_T_min  0.863
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.799
_exptl_crystal_description       block
_exptl_crystal_F_000             992
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.065
_refine_diff_density_min         -1.082
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     617
_refine_ls_number_reflns         8443
_refine_ls_number_restraints     504
_refine_ls_restrained_S_all      1.123
_refine_ls_R_factor_all          0.0702
_refine_ls_R_factor_gt           0.0447
_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^)+(0.0439P)^2^+2.3880P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1012
_refine_ls_wR_factor_ref         0.1223
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6270
_reflns_number_total             8443
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ra00684h2.cif
_cod_data_source_block           ag3p_0m_ccdc2271882
_cod_database_code               7250318
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.886
_shelx_estimated_absorpt_t_min   0.790
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 P2-F9 \\sim P2A-F9A
 with sigma of 0.02
 P2-F7 \\sim P2A-F7A
 with sigma of 0.02
 P2-F8 \\sim P2A-F8A
 with sigma of 0.02
 P2-F10 \\sim P2A-F10A
 with sigma of 0.02
 P2-F12 \\sim P2A-F12A
 with sigma of 0.02
 P2-F11 \\sim P2A-F11A
 with sigma of 0.02
 F9-F7 \\sim F9A-F7A
 with sigma of 0.04
 F9-F8 \\sim F9A-F8A
 with sigma of 0.04
 F9-F10 \\sim F9A-F10A
 with sigma of 0.04
 F9-F12 \\sim F9A-F12A
 with sigma of 0.04
 F9-F11 \\sim F9A-F11A
 with sigma of 0.04
 F7-F8 \\sim F7A-F8A
 with sigma of 0.04
 F7-F10 \\sim F7A-F10A
 with sigma of 0.04
 F7-F12 \\sim F7A-F12A
 with sigma of 0.04
 F7-F11 \\sim F7A-F11A
 with sigma of 0.04
 F8-F10 \\sim F8A-F10A
 with sigma of 0.04
 F8-F12 \\sim F8A-F12A
 with sigma of 0.04
 F8-F11 \\sim F8A-F11A
 with sigma of 0.04
 F10-F12 \\sim F10A-F12A
 with sigma of 0.04
 F10-F11 \\sim F10A-F11A
 with sigma of 0.04
 F12-F11 \\sim F12A-F11A
 with sigma of 0.04
 P1-F6 \\sim P1A-F6A
 with sigma of 0.02
 P1-F1 \\sim P1A-F1A
 with sigma of 0.02
 P1-F3 \\sim P1A-F3A
 with sigma of 0.02
 P1-F4 \\sim P1A-F4A
 with sigma of 0.02
 P1-F5 \\sim P1A-F5A
 with sigma of 0.02
 P1-F2 \\sim P1A-F2A
 with sigma of 0.02
 F6-F1 \\sim F6A-F1A
 with sigma of 0.04
 F6-F3 \\sim F6A-F3A
 with sigma of 0.04
 F6-F4 \\sim F6A-F4A
 with sigma of 0.04
 F6-F5 \\sim F6A-F5A
 with sigma of 0.04
 F6-F2 \\sim F6A-F2A
 with sigma of 0.04
 F1-F3 \\sim F1A-F3A
 with sigma of 0.04
 F1-F4 \\sim F1A-F4A
 with sigma of 0.04
 F1-F5 \\sim F1A-F5A
 with sigma of 0.04
 F1-F2 \\sim F1A-F2A
 with sigma of 0.04
 F3-F4 \\sim F3A-F4A
 with sigma of 0.04
 F3-F5 \\sim F3A-F5A
 with sigma of 0.04
 F3-F2 \\sim F3A-F2A
 with sigma of 0.04
 F4-F5 \\sim F4A-F5A
 with sigma of 0.04
 F4-F2 \\sim F4A-F2A
 with sigma of 0.04
 F5-F2 \\sim F5A-F2A
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
P2 \\sim F9 \\sim F7 \\sim F8 \\sim F10 \\sim F12 \\sim F11 \\sim F7A \\sim F8A
\\sim F9A \\sim F10A \\sim P2A \\sim F11A \\sim F12A: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2A
P1 \\sim F1 \\sim F3 \\sim F4 \\sim F5 \\sim F2 \\sim F2A \\sim F3A \\sim F6A
\\sim F5A \\sim P1A \\sim F1A \\sim F4A \\sim F6: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.02 within 2A
4. Others
 Sof(F7A)=Sof(F8A)=Sof(F9A)=Sof(F10A)=Sof(P2A)=Sof(F11A)=Sof(F12A)=1-FVAR(1)
 Sof(P2)=Sof(F9)=Sof(F7)=Sof(F8)=Sof(F10)=Sof(F12)=Sof(F11)=FVAR(1)
 Sof(F2A)=Sof(F3A)=Sof(F6A)=Sof(F5A)=Sof(P1A)=Sof(F1A)=Sof(F4A)=1-FVAR(2)
 Sof(P1)=Sof(F6)=Sof(F1)=Sof(F3)=Sof(F4)=Sof(F5)=Sof(F2)=FVAR(2)
5.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C21(H21A,H21B)
5.b Aromatic/amide H refined with riding coordinates:
 C20(H20), C2(H2), C26(H26), C7(H7), C15(H15), C3(H3), C13(H13), C18(H18),
 C23(H23), C16(H16), C10(H10), C17(H17), C5(H5), C4(H4), C11(H11), C12(H12),
 C25(H25), C24(H24)
5.c Idealised Me refined as rotating group:
 C28(H28A,H28B,H28C), C30(H30A,H30B,H30C)
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_shelx_res_checksum              22334
_olex2_submission_special_instructions 'No special instructions were received'