Synthesis, X-ray Characterization and DFT analysis of Dicyanidoaurate Telluronium salts: on the importance of charge assisted chalcogen bonds
Ghinato, Simone; Giordana, Alessia; Diana, Eliano; Gomila, Rosa Maria; Priola, Emanuele; Frontera, Antonio; Dalton Transactions  (2023) –; doi:10.1039/D3DT02787B

data_7714183
_publ_section_title
;
 Synthesis, X-ray Characterization and DFT analysis of Dicyanidoaurate
 Telluronium salts: on the importance of charge assisted chalcogen bonds
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT02787B
_journal_year                    2023
_chemical_formula_moiety         'C13 H13 Te, Au C2 N2'
_chemical_formula_sum            'C15 H13 Au N2 Te'
_chemical_formula_weight         545.84
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_audit_creation_date             2023-06-28
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-07-24 deposited with the CCDC.	2023-10-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.514(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.2490(2)
_cell_length_b                   13.2961(2)
_cell_length_c                   13.4912(3)
_cell_measurement_reflns_used    9674
_cell_measurement_temperature    298.00
_cell_measurement_theta_max      66.5610
_cell_measurement_theta_min      5.0650
_cell_volume                     1573.22(6)
_computing_cell_refinement       'CrysAlisPro 1.171.42.53a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.53a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.53a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (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 0.977
_diffrn_measured_fraction_theta_max 0.977
_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     24.00 114.00   1.00   30.00    --   42.89  57.00  60.00   90
  2  \w    -10.00  71.00   1.00   30.00    --   42.89 -57.00 120.00   81
  3  \w    -23.00  70.00   1.00   30.00    --   42.89 -57.00 -90.00   93
  4  \w     73.00  99.00   1.00   30.00    --   92.50 -70.00 150.76   26
  5  \w     88.00 114.00   1.00   30.00    --   92.50  61.00  30.00   26
  6  \w     81.00 107.00   1.00   30.00    --   92.50 -30.00-120.00   26
  7  \w     55.00  99.00   1.00   30.00    --   92.50 -70.00  52.53   44
  8  \w     17.00  43.00   1.00   30.00    --   92.50 -30.00  90.00   26
  9  \w     60.00  86.00   1.00   30.00    --   92.50 -30.00  90.00   26
 10  \w    127.00 153.00   1.00   30.00    --   92.50  15.00  30.00   26
 11  \w     25.00  99.00   1.00   30.00    --   92.50 -70.00-122.83   74
 12  \w     16.00  52.00   1.00   30.00    --   92.50 -15.00  30.00   36
 13  \w    112.00 143.00   1.00   30.00    --   92.50  45.00 -30.00   31
 14  \w     21.00 110.00   1.00   30.00    --   92.50 -70.00 -61.51   89
 15  \w     41.00 174.00   1.00   30.00    --   92.50  15.00 -60.00  133
 16  \w     77.00 156.00   1.00   30.00    --   92.50  61.00 150.00   79
 17  \w     20.00  51.00   1.00   30.00    --   92.50 -70.00 100.78   31
 18  \w     70.00 121.00   1.00   30.00    --   92.50 -70.00 100.78   51
 19  \w     38.00  97.00   1.00   30.00    --   92.50 -69.00-156.95   59
 20  \w     59.00  85.00   1.00   30.00    --   92.50  15.00  30.00   26
 21  \w    111.00 154.00   1.00   30.00    --   92.50  45.00-180.00   43
 22  \w     65.00  98.00   1.00   30.00    --   92.50 -30.00-180.00   33
 23  \w     80.00 105.00   1.00   30.00    --   92.50 -70.00 -13.92   25
 24  \w     27.00  53.00   1.00   30.00    --   92.50 -61.00 -60.00   26
 25  \w     84.00 120.00   1.00   30.00    --   92.50 -61.00 -60.00   36
 26  \w     80.00 106.00   1.00   30.00    --   92.50  15.00 120.00   26
 27  \w     19.00  49.00   1.00   30.00    --   92.50 -70.00  52.53   30
 28  \w     49.00  75.00   1.00   30.00    --   92.50 -70.00 138.46   26
 29  \w     78.00 109.00   1.00   30.00    --   92.50  45.00-150.00   31
 30  \w     72.00 137.00   1.00   30.00    --   92.50  45.00  30.00   65
 31  \w     31.00 121.00   1.00   30.00    --   92.50 -70.00  78.11   90
 32  \w     30.00  55.00   1.00   30.00    --   92.50 -61.00-150.00   25
 33  \w     72.00  98.00   1.00   30.00    --   92.50 -70.00  17.33   26
;
_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      -0.0086999000
_diffrn_orient_matrix_UB_12      0.0755248000
_diffrn_orient_matrix_UB_13      0.0845945000
_diffrn_orient_matrix_UB_21      0.0014614000
_diffrn_orient_matrix_UB_22      0.0878813000
_diffrn_orient_matrix_UB_23      -0.0741477000
_diffrn_orient_matrix_UB_31      -0.1752963000
_diffrn_orient_matrix_UB_32      -0.0029827000
_diffrn_orient_matrix_UB_33      -0.0430341000
_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  0.0529
_diffrn_reflns_av_unetI/netI     0.0244
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            16022
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        66.791
_diffrn_reflns_theta_max         66.791
_diffrn_reflns_theta_min         4.797
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    31.808
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.06702
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.53a (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    2.305
_exptl_crystal_description       block
_exptl_crystal_F_000             992
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Ethanol'
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.7
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.321
_refine_diff_density_min         -1.986
_refine_diff_density_rms         0.179
_refine_ls_extinction_coef       0.00077(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     174
_refine_ls_number_reflns         2725
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0425
_refine_ls_R_factor_gt           0.0400
_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^)+(0.0748P)^2^+1.1180P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1075
_refine_ls_wR_factor_ref         0.1108
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2478
_reflns_number_total             2725
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02787b2.cif
_cod_data_source_block           preex1
_cod_original_cell_volume        1573.21(6)
_cod_database_code               7714183
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C11 H10 N O'
_shelx_estimated_absorpt_t_max   0.115
_shelx_estimated_absorpt_t_min   0.015
_olex2_refinement_description
;
1.a Aromatic/amide H refined with riding coordinates:
 C9(H9), C8(H8), C11(H11), C15(H15), C5(H5), C6(H6), C7(H7), C14(H14),
 C13(H13), C12(H12)
1.b Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C)
;
_shelx_res_checksum              17756
_olex2_date_sample_data_collection 2022-10-12
_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 6.949
_oxdiff_exptl_absorpt_empirical_full_min 0.466