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_7249996
_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), C15 H17 N3 O3 Zn'
_chemical_formula_sum            'C23 H17 Au2 N11 O3 Zn'
_chemical_formula_weight         954.78
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2023-11-17
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   27.7951(10)
_cell_length_b                   19.2710(7)
_cell_length_c                   7.8649(2)
_cell_measurement_reflns_used    3610
_cell_measurement_temperature    298.00
_cell_measurement_theta_max      66.5490
_cell_measurement_theta_min      2.7650
_cell_volume                     4212.8(2)
_computing_cell_refinement       'CrysAlisPro 1.171.42.101a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.101a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.101a (Rigaku OD, 2023)'
_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      298.00
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1990
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_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     -6.00  19.00   1.00   20.00    --   42.89 -34.00  46.00   25
  2  \w     18.00  78.00   1.00   20.00    --   42.89  34.00-155.00   60
  3  \w     94.00 119.00   1.00   20.00    --   92.50  34.00-155.00   25
  4  \w     32.00  83.00   1.00   20.00    --   92.50 -34.00  46.00   51
  5  \w     35.00 117.00   1.00   20.00    --   42.89  37.00 -60.00   82
  6  \w    111.00 137.00   1.00   20.00    --   92.50  70.00 -23.44   26
  7  \w     79.00 122.00   1.00   20.00    --   92.50 -61.00   0.00   43
  8  \w     20.00  55.00   1.00   20.00    --   92.50 -45.00   0.00   35
  9  \w     26.00  56.00   1.00   20.00    --   92.50 -45.00  30.00   30
 10  \w     25.00  51.00   1.00   20.00    --   92.50 -61.00   0.00   26
 11  \w     59.00 116.00   1.00   20.00    --   92.50 -69.00-139.06   57
 12  \w     23.00  51.00   1.00   20.00    --   92.50 -45.00-120.00   28
 13  \w     90.00 118.00   1.00   20.00    --   92.50 -45.00-120.00   28
;
_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      -0.0131104000
_diffrn_orient_matrix_UB_12      -0.0749662000
_diffrn_orient_matrix_UB_13      -0.0497793000
_diffrn_orient_matrix_UB_21      -0.0513491000
_diffrn_orient_matrix_UB_22      0.0110957000
_diffrn_orient_matrix_UB_23      0.0683706000
_diffrn_orient_matrix_UB_31      -0.0161706000
_diffrn_orient_matrix_UB_32      0.0254582000
_diffrn_orient_matrix_UB_33      -0.1767378000
_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  0.1323
_diffrn_reflns_av_unetI/netI     0.0719
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            12823
_diffrn_reflns_point_group_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        66.843
_diffrn_reflns_theta_max         66.843
_diffrn_reflns_theta_min         2.790
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    13.766
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.46272
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.101a (Rigaku Oxford Diffraction, 2023)
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    1.505
_exptl_crystal_description       needle
_exptl_crystal_F_000             1776
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.691
_refine_diff_density_min         -2.724
_refine_diff_density_rms         0.248
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     187
_refine_ls_number_reflns         3657
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0840
_refine_ls_R_factor_gt           0.0667
_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^)+(0.1085P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1845
_refine_ls_wR_factor_ref         0.2073
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2492
_reflns_number_total             3657
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cp04818k2.cif
_cod_data_source_block           preex5_auto
_cod_database_code               7249996
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.683
_shelx_estimated_absorpt_t_min   0.446
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 Zn1-H1A \\sim Zn1-H1B
 with sigma of 0.02
3. Others
 Fixed Sof: H2A(0.5) H2B(0.5)
4.a Free rotating group:
 O1(H1A,H1B)
4.b Rotating group:
 O2(H2A,H2B)
4.c Aromatic/amide H refined with riding coordinates:
 C7(H7), C12(H12), C8(H8), C5(H5), C6(H6), C11(H11)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 490 electrons were 
found in a volume of 1586\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
2[C3N1O1H7] per Asymmetric Unit 
which account for 320 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              43767
_shelx_fab_checksum              78984
_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 2.978
_oxdiff_exptl_absorpt_empirical_full_min 0.266