Exploring Coinage Bonding Interactions in [Au(CN)₄]⁻ Assemblies with Silver and Zinc Complexes: A Structural and Theoretical Study
Giordana, Alessia; Priola, Emanuele; Mahmoudi, Ghodrat; Doustkhah, Esmail; Gomila, Rosa Maria; Zangrando, Ennio; Diana, Eliano; Operti, Lorenza; Frontera, Antonio; Physical Chemistry Chemical Physics  (2024) –; doi:10.1039/D4CP04818K

data_7249999
_publ_section_title
;
 Exploring Coinage Bonding Interactions in [Au(CN)&#x2084;]&#x207B;
 Assemblies with Silver and Zinc Complexes: A Structural and Theoretical
 Study
;
_journal_name_full               'Physical Chemistry Chemical Physics'
_journal_paper_doi               10.1039/D4CP04818K
_journal_year                    2024
_chemical_formula_moiety         '2(Au C4 N4), C30 H24 N6 Zn'
_chemical_formula_sum            'C38 H24 Au2 N14 Zn'
_chemical_formula_weight         1136.01
_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     direct
_audit_creation_date             2023-08-03
_audit_creation_method
;
Olex2 1.5-ac5-024
(compiled 2022.04.12 svn.rca3783a0 for Rigaku Oxford Diffraction, GUI svn.r6498)
;
_audit_update_record
;
2024-10-19 deposited with the CCDC.	2025-02-19 downloaded from the CCDC.
;
_cell_angle_alpha                84.0567(17)
_cell_angle_beta                 88.165(2)
_cell_angle_gamma                80.659(2)
_cell_formula_units_Z            4
_cell_length_a                   8.9756(3)
_cell_length_b                   11.2053(2)
_cell_length_c                   41.1536(9)
_cell_measurement_reflns_used    17926
_cell_measurement_temperature    293
_cell_measurement_theta_max      66.5650
_cell_measurement_theta_min      3.9940
_cell_volume                     4061.67(18)
_computing_cell_refinement       'CrysAlisPro 1.171.42.71a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.71a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.71a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      293
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1990
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.967
_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     18.00 115.00   1.00   20.00    --   42.89  57.00 -60.00   97
  2  \w    -26.00  66.00   1.00   20.00    --   42.89 -57.00 150.00   92
  3  \w     -5.00  70.00   1.00   20.00    --   42.89 -57.00   0.00   75
  4  \w     31.00  57.00   1.00   20.00    --   92.50 -30.00  90.00   26
  5  \w     19.00  65.00   1.00   20.00    --   92.50 -70.00 -54.06   46
  6  \w     67.00  93.00   1.00   20.00    --   92.50 -70.00 127.58   26
  7  \w    101.00 127.00   1.00   20.00    --   92.50  30.00  90.00   26
  8  \w     67.00  94.00   1.00   20.00    --   92.50  45.00 -30.00   27
  9  \w     65.00 123.00   1.00   20.00    --   92.50 -15.00 120.00   58
 10  \w     19.00 123.00   1.00   20.00    --   92.50 -70.00  75.33  104
 11  \w    109.00 173.00   1.00   20.00    --   92.50  15.00  60.00   64
 12  \w     71.00  97.00   1.00   20.00    --   92.50 -70.00 -54.06   26
 13  \w     86.00 112.00   1.00   20.00    --   92.50  30.00 -60.00   26
 14  \w    136.00 169.00   1.00   20.00    --   92.50  30.00 -60.00   33
 15  \w     45.00 100.00   1.00   20.00    --   92.50 -70.00  36.72   55
 16  \w     91.00 118.00   1.00   20.00    --   92.50 -70.00  93.23   27
 17  \w     91.00 118.00   1.00   20.00    --   92.50 -45.00 120.00   27
 18  \w     50.00 101.00   1.00   20.00    --   92.50 -70.00 -12.74   51
 19  \w     20.00  51.00   1.00   20.00    --   92.50 -45.00  30.00   31
 20  \w     79.00 104.00   1.00   20.00    --   92.50  61.00 -90.00   25
 21  \w    122.00 159.00   1.00   20.00    --   92.50  61.00 -90.00   37
 22  \w     41.00  96.00   1.00   20.00    --   92.50  15.00  60.00   55
 23  \w     66.00 115.00   1.00   20.00    --   92.50  61.00-180.00   49
 24  \w     38.00  85.00   1.00   20.00    --   92.50 -45.00   0.00   47
 25  \w     33.00  59.00   1.00   20.00    --   92.50 -70.00 -60.70   26
 26  \w     74.00  99.00   1.00   20.00    --   92.50 -70.00 -60.70   25
 27  \w     19.00 109.00   1.00   20.00    --   92.50 -70.00 179.34   90
 28  \w     70.00  95.00   1.00   20.00    --   92.50  30.00 -30.00   25
 29  \w    130.00 156.00   1.00   20.00    --   92.50  30.00 -30.00   26
 30  \w     38.00  63.00   1.00   20.00    --   92.50 -34.00 118.00   25
 31  \w     79.00 106.00   1.00   20.00    --   92.50 -34.00 118.00   27
 32  \w    129.00 156.00   1.00   20.00    --   92.50  30.00-180.00   27
 33  \w     29.00  55.00   1.00   20.00    --   92.50 -70.00   2.20   26
 34  \w     90.00 116.00   1.00   20.00    --   92.50 -70.00   2.20   26
 35  \w     52.00 112.00   1.00   20.00    --   92.50  17.00-155.29   60
 36  \w    132.00 163.00   1.00   20.00    --   92.50  17.00-155.29   31
 37  \w     19.00  54.00   1.00   20.00    --   92.50 -45.00 -60.00   35
 38  \w     80.00 105.00   1.00   20.00    --   92.50 -45.00 -60.00   25
 39  \w     90.00 121.00   1.00   20.00    --   92.50 -30.00  90.00   31
 40  \w     35.00  60.00   1.00   20.00    --   92.50 -48.00  53.51   25
 41  \w     79.00 114.00   1.00   20.00    --   92.50 -48.00  53.51   35
 42  \w     30.00  55.00   1.00   20.00    --   92.50 -69.00 -76.28   25
 43  \w     67.00  96.00   1.00   20.00    --   92.50  45.00 150.00   29
 44  \w     63.00  88.00   1.00   20.00    --   92.50 -51.00 129.16   25
 45  \w     41.00  67.00   1.00   20.00    --   92.50 -33.00 -97.26   26
 46  \w     79.00 117.00   1.00   20.00    --   92.50 -33.00 -97.26   38
 47  \w     79.00 120.00   1.00   20.00    --   92.50 -70.00-116.71   41
 48  \w    122.00 147.00   1.00   20.00    --   92.50  61.00-120.00   25
 49  \w     56.00  99.00   1.00   20.00    --   92.50 -70.00-148.81   43
 50  \w     60.00 100.00   1.00   20.00    --   92.50 -70.00 -98.26   40
 51  \w     61.00  86.00   1.00   20.00    --   92.50 -70.00  29.25   25
 52  \w     17.00  42.00   1.00   20.00    --   92.50 -30.00-120.00   25
 53  \w     23.00  48.00   1.00   20.00    --   92.50 -70.00-116.71   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, AtlasS2, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0165596000
_diffrn_orient_matrix_UB_12      0.0189548000
_diffrn_orient_matrix_UB_13      0.0361743000
_diffrn_orient_matrix_UB_21      -0.1719462000
_diffrn_orient_matrix_UB_22      0.0403876000
_diffrn_orient_matrix_UB_23      0.0028759000
_diffrn_orient_matrix_UB_31      -0.0206001000
_diffrn_orient_matrix_UB_32      -0.1327334000
_diffrn_orient_matrix_UB_33      0.0100008000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0503
_diffrn_reflns_av_unetI/netI     0.0348
_diffrn_reflns_Laue_measured_fraction_full 0.967
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       -49
_diffrn_reflns_number            58197
_diffrn_reflns_point_group_measured_fraction_full 0.967
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        66.993
_diffrn_reflns_theta_max         66.993
_diffrn_reflns_theta_min         3.239
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    14.373
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.37259
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.71a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.858
_exptl_crystal_description       plate
_exptl_crystal_F_000             2152
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.625
_refine_diff_density_min         -1.458
_refine_diff_density_rms         0.087
_refine_ls_extinction_coef       0.000099(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     992
_refine_ls_number_reflns         14027
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0452
_refine_ls_R_factor_gt           0.0357
_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^)+(0.0329P)^2^+2.9533P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0781
_refine_ls_wR_factor_ref         0.0831
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11815
_reflns_number_total             14027
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cp04818k2.cif
_cod_data_source_block           preex1_auto_CCDC1
_cod_original_cell_volume        4061.69(17)
_cod_database_code               7249999
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C11 H10 N O'
_shelx_estimated_absorpt_t_max   0.762
_shelx_estimated_absorpt_t_min   0.479
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C25(H25), C47(H47), C68(H68), C17(H17), C46(H46), C56(H56), C38(H38),
 C20(H20), C66(H66), C55(H55), C57(H57), C65(H65), C37(H37), C60(H60), C28(H28),
  C35(H35), C74(H74), C24(H24), C53(H53), C36(H36), C75(H75), C23(H23),
 C64(H64), C43(H43), C26(H26), C27(H27), C67(H67), C76(H76), C33(H33), C45(H45),
  C54(H54), C18(H18), C48(H48), C19(H19), C70(H70), C69(H69), C40(H40),
 C59(H59), C39(H39), C63(H63), C44(H44), C58(H58), C34(H34), C29(H29), C73(H73),
  C49(H49), C50(H50), C30(H30)
;
_shelx_res_checksum              5929
_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 2.501
_oxdiff_exptl_absorpt_empirical_full_min 0.654