Unexpected structural preference with metallophilic Ag-Au contacts in silver(I)-N-heterocyclic carbene cluster; experimental and theoretical approach.
Sahu, Priyanka; Jana, Narayan Ch; Barik, Sahadev; Kisan, Hemanta K.; Changotra, Avtar; Isab, Anvarhusein A.; Dinda, Joydev; Dalton transactions (Cambridge, England : 2003) 53 (2024) 1099–1104; doi:10.1039/d3dt02551a

data_7714747
_publ_section_title
;
 Unexpected structural preference with metallophilic Ag-Au contacts in
 silver(I)-N-heterocyclic carbene cluster; experimental and theoretical
 approach.
;
_journal_issue                   3
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1099
_journal_page_last               1104
_journal_paper_doi               10.1039/d3dt02551a
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C63 H60 Ag3 N18, 3(F6 P1), 0.5(C4 H4 N2)'
_chemical_formula_sum            'C65 H62 Ag3 F18 N19 P3'
_chemical_formula_weight         1867.85
_space_group_crystal_system      trigonal
_space_group_IT_number           165
_space_group_name_Hall           '-P 3 2"c'
_space_group_name_H-M_alt        'P -3 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-12-03
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2023-04-26 deposited with the CCDC.	2023-12-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   23.0541(3)
_cell_length_b                   23.0541(3)
_cell_length_c                   23.7591(4)
_cell_measurement_reflns_used    34615
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      30.6820
_cell_measurement_theta_min      1.9630
_cell_volume                     10936.0(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_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      100.01(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.854
_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    -72.00  -1.00   0.50   80.18    --   -4.29 -31.00 -59.00  142
  2  \w      1.00  67.00   0.50   80.18    --    3.67  37.00 150.00  132
  3  \w     -8.00  55.00   0.50   80.18    --    3.67  57.00   0.00  126
  4  \w    -14.00  27.00   0.50   80.18    --   -4.29 -99.00-150.00   82
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Dual, Cu at home/near, Pilatus 200K'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0325015000
_diffrn_orient_matrix_UB_12      -0.0205809000
_diffrn_orient_matrix_UB_13      0.0112946000
_diffrn_orient_matrix_UB_21      -0.0033959000
_diffrn_orient_matrix_UB_22      0.0286467000
_diffrn_orient_matrix_UB_23      0.0040922000
_diffrn_orient_matrix_UB_31      -0.0139304000
_diffrn_orient_matrix_UB_32      -0.0042117000
_diffrn_orient_matrix_UB_33      -0.0273216000
_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  0.0345
_diffrn_reflns_av_unetI/netI     0.0183
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.854
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            81962
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.854
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.589
_diffrn_reflns_theta_min         1.964
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.965
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.52328
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            white
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    1.702
_exptl_crystal_description       block
_exptl_crystal_F_000             5598
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.207
_refine_diff_density_min         -0.865
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     501
_refine_ls_number_reflns         9586
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0413
_refine_ls_R_factor_gt           0.0324
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0319P)^2^+21.7346P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0760
_refine_ls_wR_factor_ref         0.0813
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8104
_reflns_number_total             9586
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02551a2.cif
_cod_data_source_block           sdv_ptcomplex
_cod_depositor_comments
'Adding full bibliography for 7714747--7714748.cif.'
_cod_database_code               7714747
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N P F Ag'
_shelx_estimated_absorpt_t_max   0.910
_shelx_estimated_absorpt_t_min   0.830
_reflns_odcompleteness_completeness 99.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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. Others
 Fixed Sof: N10(0.5) H33A(0.5) H33B(0.5) C34(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C30(H30A,H30B), C9(H9A,H9B), C13(H13A,H13B), C33(H33A,H33B)
3.b Aromatic/amide H refined with riding coordinates:
 C32(H32), C10(H10), C11(H11), C16(H16), C2(H2), C19(H19), C23(H23), C17(H17),
 C18(H18), C26(H26), C3(H3), C5(H5), C24(H24), C4(H4), C25(H25)
3.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C29(H29A,H29B,H29C), C21(H21A,H21B,H21C)
;
_shelx_res_checksum              54846
_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 1.493
_oxdiff_exptl_absorpt_empirical_full_min 0.637