Isolation of mixed valence charge-neutral Ag<sub>12</sub>, and dicationic Ag<sub>10</sub> nano-clusters stabilized by carbene-phosphaalkenides.
Francis, Maria; Patra, Asutosh; Salam, Farsana Abdul; Prathapa, Siriyara Jagannatha; Roy, Sudipta; Chemical communications (Cambridge, England) 61 (2025) 1379–1382; doi:10.1039/d4cc05628k

data_7134188
_publ_section_title
;
 Isolation of mixed valence charge-neutral Ag<sub>12</sub>, and dicationic
 Ag<sub>10</sub> nano-clusters stabilized by carbene-phosphaalkenides.
;
_journal_issue                   7
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              1379
_journal_page_last               1382
_journal_paper_doi               10.1039/d4cc05628k
_journal_volume                  61
_journal_year                    2025
_chemical_formula_moiety         'C120 H186 Ag12 Cl3 N6 P6'
_chemical_formula_sum            'C120 H186 Ag12 Cl3 N6 P6'
_chemical_formula_weight         3299.35
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2023-01-18
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2024-10-19 deposited with the CCDC.	2024-12-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   32.5258(13)
_cell_length_b                   32.5258(13)
_cell_length_c                   16.6904(10)
_cell_measurement_reflns_used    9736
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.59
_cell_measurement_theta_min      2.17
_cell_volume                     15291.6(13)
_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  'XL  (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.00
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_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  0.0514
_diffrn_reflns_av_unetI/netI     0.0128
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            211782
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.403
_diffrn_reflns_theta_min         1.892
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.240
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6429
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0733 before and 0.0550 after correction.
The Ratio of minimum to maximum transmission is 0.8625.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.075
_exptl_crystal_description       block
_exptl_crystal_F_000             4959
_exptl_crystal_size_max          0.081
_exptl_crystal_size_mid          0.072
_exptl_crystal_size_min          0.067
_refine_diff_density_max         1.671
_refine_diff_density_min         -1.644
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.134
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     230
_refine_ls_number_reflns         6982
_refine_ls_number_restraints     51
_refine_ls_restrained_S_all      1.159
_refine_ls_R_factor_all          0.1025
_refine_ls_R_factor_gt           0.0832
_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^)+(0.1302P)^2^+84.2387P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2523
_refine_ls_wR_factor_ref         0.2759
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4867
_reflns_number_total             6982
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc05628k2.cif
_cod_data_source_block           mo_sr1223_0m_a
_cod_original_cell_volume        15291.6(15)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               7134188
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_max   0.922
_shelx_estimated_absorpt_t_min   0.906
_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. Rigid bond restraints
 P2, Cl2, Cl1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C7, C16, C15
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C9, C18, C17
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C4, C15, C16, C17, C18
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 P2, Ag1
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
3. Uiso/Uaniso restraints and constraints
Ag2 \\sim Cl2 \\sim Cl1: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
C7 \\sim C16 \\sim C15: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
C9 \\sim C17 \\sim C18: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
C1 \\sim C16 \\sim C15: within 2A with sigma of 0.001 and sigma for terminal
atoms of 0.002 within 2A
P2 \\sim Ag1: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
Uanis(C17) \\sim Ueq, Uanis(C18) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.01
Uanis(Ag1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 P2, Ag1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5.a Ternary CH refined with riding coordinates:
 C11(H11), C13(H13)
5.b Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5)
5.d Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,
 H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,
 H20B,H20C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.4
_shelx_res_checksum              20313
_shelx_hkl_checksum              89718
_shelx_fab_checksum              77319
_olex2_submission_special_instructions 'No special instructions were received'