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_7714748
_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
'C42 H40 Ag2 Au Cl N12, 2(F6 P), C2.5 H5 N O0.5'
_chemical_formula_sum            'C44.5 H45 Ag2 Au Cl F12 N13 O0.5 P2'
_chemical_formula_weight         1508.03
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-I 2y'
_space_group_name_H-M_alt        'I 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-12-13
_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                 96.862(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.2719(4)
_cell_length_b                   24.7697(6)
_cell_length_c                   14.7213(4)
_cell_measurement_reflns_used    14497
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      30.6130
_cell_measurement_theta_min      3.7680
_cell_volume                     5166.9(2)
_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(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.819
_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    -65.00   7.00   0.50   23.71    --    3.35 -24.00 121.00  144
  2  \w      0.00  73.00   0.50   23.71    --    3.35  24.00 -74.00  146
  3  \w    -15.00  39.00   0.50   23.71    --    3.35 -99.00 -90.00  108
  4  \w     -5.00  23.00   0.50   23.71    --   -4.29 -99.00-180.00   56
  5  \w    -27.00   7.00   0.50   23.71    --   -4.29  77.00  60.00   68
  6  \w    -24.00  18.00   0.50   23.71    --   -4.29 -77.00-120.00   84
  7  \w    -25.00  11.00   0.50   23.71    --   -4.29  77.00   0.00   72
  8  \w     -3.00  30.00   0.50   23.71    --   -4.29 -99.00   0.00   66
;
_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      -0.0447157000
_diffrn_orient_matrix_UB_12      -0.0082127000
_diffrn_orient_matrix_UB_13      -0.0218735000
_diffrn_orient_matrix_UB_21      0.0197072000
_diffrn_orient_matrix_UB_22      -0.0036233000
_diffrn_orient_matrix_UB_23      -0.0415693000
_diffrn_orient_matrix_UB_31      0.0108884000
_diffrn_orient_matrix_UB_32      -0.0271984000
_diffrn_orient_matrix_UB_33      0.0121378000
_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  0.0750
_diffrn_reflns_av_unetI/netI     0.0573
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.819
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            30536
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.819
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.330
_diffrn_reflns_theta_min         3.313
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.789
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61963
_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            'clear light silver'
_exptl_crystal_density_diffrn    1.939
_exptl_crystal_description       block
_exptl_crystal_F_000             2940
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.001
_refine_diff_density_min         -1.226
_refine_diff_density_rms         0.164
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     380
_refine_ls_number_reflns         6503
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0529
_refine_ls_R_factor_gt           0.0427
_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^)+(0.0256P)^2^+49.6891P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0927
_refine_ls_wR_factor_ref         0.0959
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5596
_reflns_number_total             6503
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02551a2.cif
_cod_data_source_block           jd-3_r2
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_diffrn_ambient_temperature' value '100.00 (10)' was
changed to '100(10)' -- precision was estimated.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 

 Adding full bibliography for 7714747--7714748.cif.
;
_cod_original_formula_sum        'C44.50 H45 Ag2 Au Cl F12 N13 O0.50 P2'
_cod_database_code               7714748
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N O Ag Au P F Cl'
_shelx_estimated_absorpt_t_max   0.703
_shelx_estimated_absorpt_t_min   0.518
_reflns_odcompleteness_completeness 99.54
_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. Restrained distances
 N7-C24
 1.3 with sigma of 0.02
3. Others
 Fixed Sof: F9(0.85) O1(0.25) C24(0.25) C23(0.5) H23A(0.5) H23B(0.5) H23C(0.5)
 C22(0.5) H22A(0.5) H22B(0.5) F8(0.15)
4.a Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C9(H9A,H9B), C22(H22A,H22B)
4.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C19(H19), C18(H18), C16(H16), C2(H2), C17(H17), C11(H11), C4(H4),
 C3(H3), C5(H5)
4.c Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C7(H7A,H7B,H7C), C23(H23A,H23B,H23C)
;
_shelx_res_checksum              15492
_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 2.108
_oxdiff_exptl_absorpt_empirical_full_min 0.195