Antibacterial silver and gold complexes of imidazole and 1,2,4-triazole derived N-heterocyclic carbenes
Barnard, Peter; Mather , Joel; Wyllie, Jessica Anne; Hamilton, Alex; Soares da Costa, Tatiana P.; Dalton Transactions  (2022) –; doi:10.1039/D2DT01657E

data_7710764
_publ_section_title
;
 Antibacterial silver and gold complexes of imidazole and 1,2,4-triazole
 derived N-heterocyclic carbenes
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT01657E
_journal_year                    2022
_chemical_formula_moiety         'C22 H24 Au N4, I'
_chemical_formula_sum            'C22 H24 Au I N4'
_chemical_formula_weight         668.32
_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     dual
_audit_creation_date             2021-10-26
_audit_creation_method
;
Olex2 1.5
(compiled 2021.10.07 svn.r9718050b for OlexSys, GUI svn.r6410)
;
_audit_update_record
;
2022-05-19 deposited with the CCDC.	2022-07-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.2300(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.89520(10)
_cell_length_b                   17.19070(10)
_cell_length_c                   13.18180(10)
_cell_measurement_reflns_used    12422
_cell_measurement_temperature    149.99(10)
_cell_measurement_theta_max      64.6480
_cell_measurement_theta_min      4.2260
_cell_volume                     2242.28(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_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    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      149.99(10)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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    -63.00  -8.00   0.50    0.20    --    0.00 -72.00 138.00  110
  2  \w     -4.00  21.00   0.50    0.20    --    0.00 -72.00 138.00   50
  3  \w     46.00 104.00   0.50    0.62    --   86.16 -72.00 138.00  116
  4  \w     67.00 149.00   0.50    0.62    --   86.16  72.00 -91.00  164
  5  \w    -67.00 -34.00   0.50    0.20    --    0.00 -19.00  30.00   66
  6  \w    -29.00   7.00   0.50    0.20    --    0.00 -19.00  30.00   72
  7  \w    -18.00  32.00   0.50    0.20    --    0.00  77.00 -60.00  100
  8  \w    -22.00  37.00   0.50    0.20    --    0.00  77.00  30.00  118
  9  \w     33.00  68.00   0.50    0.20    --    0.00  19.00-150.00   70
 10  \w      3.00  28.00   0.50    0.20    --    0.00  19.00-150.00   50
 11  \w    -19.00   7.00   0.50    0.20    --    0.00  77.00-120.00   52
 12  \w     38.00  63.00   0.50    0.20    --    0.00  72.00 -91.00   50
 13  \w     -8.00  34.00   0.50    0.20    --    0.00  38.00 -90.00   84
 14  \w    -23.00  19.00   0.50    0.20    --    0.00  77.00  90.00   84
 15  \w     38.00 117.00   0.50    0.62    --   86.16-145.00 -30.00  158
 16  \w     92.00 144.00   0.50    0.62    --   86.16  28.00 -30.00  104
 17  \w    117.00 143.00   0.50    0.62    --   86.16  96.00  30.00   52
 18  \w     69.00 106.00   0.50    0.62    --   86.16  67.00 150.00   74
 19  \w    121.00 147.00   0.50    0.62    --   86.16 117.00 120.00   52
 20  \w     48.00 101.00   0.50    0.62    --   86.16 -57.00   0.00  106
 21  \w    106.00 135.00   0.50    0.62    --   86.16  77.00-150.00   58
 22  \w     38.00  83.00   0.50    0.62    --   86.16 -47.00 150.00   90
 23  \w     86.00 146.00   0.50    0.62    --   86.16  47.00  60.00  120
 24  \w     26.00  89.00   0.50    0.62    --   86.16-117.00 150.00  126
 25  \w     25.00  51.00   0.50    0.62    --   86.16-117.00-180.00   52
 26  \w     84.00 109.00   0.50    0.62    --   86.16-117.00-180.00   50
 27  \w     31.00 107.00   0.50    0.62    --   86.16-117.00 -30.00  152
 28  \w    102.00 147.00   0.50    0.62    --   86.16 117.00 150.00   90
 29  \w     16.00  92.00   0.50    0.62    --   86.16 -19.00 120.00  152
 30  \w     65.00 109.00   0.50    0.62    --   86.16 -77.00  90.00   88
 31  \w    103.00 138.00   0.50    0.62    --   86.16 117.00-180.00   70
 32  \w     51.00  83.00   0.50    0.62    --   86.16-145.00 -60.00   64
 33  \w    102.00 127.00   0.50    0.62    --   86.16-145.00 -60.00   50
 34  \w    103.00 149.00   0.50    0.62    --   86.16 117.00  90.00   92
 35  \w    107.00 141.00   0.50    0.62    --   86.16  77.00-180.00   68
 36  \w    118.00 144.00   0.50    0.62    --   86.16 117.00 -60.00   52
 37  \w     43.00 110.00   0.50    0.62    --   86.16 -88.00   0.00  134
 38  \w     74.00 106.00   0.50    0.62    --   86.16-117.00  90.00   64
 39  \w    121.00 147.00   0.50    0.62    --   86.16  67.00 150.00   52
 40  \w     70.00 145.00   0.50    0.62    --   86.16  57.00  90.00  150
 41  \w     33.00  97.00   0.50    0.62    --   86.16 -96.00 -30.00  128
 42  \w     22.00  87.00   0.50    0.62    --   86.16 -28.00 -90.00  130
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, HyPix3000'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0278
_diffrn_reflns_av_unetI/netI     0.0197
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            16824
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        64.743
_diffrn_reflns_theta_max         64.743
_diffrn_reflns_theta_min         4.226
_exptl_absorpt_coefficient_mu    23.242
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.41177
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.980
_exptl_crystal_description       block
_exptl_crystal_F_000             1264
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.619
_refine_diff_density_min         -0.934
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     255
_refine_ls_number_reflns         3783
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0191
_refine_ls_R_factor_gt           0.0182
_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^)+(0.0242P)^2^+1.7144P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0454
_refine_ls_wR_factor_ref         0.0460
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3664
_reflns_number_total             3783
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01657e2.cif
_cod_data_source_block           4b
_cod_database_code               7710764
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.457
_shelx_estimated_absorpt_t_min   0.389
_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.a Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C21(H21A,H21B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9), C13(H13), C14(H14),
 C16(H16), C17(H17), C18(H18), C19(H19), C20(H20)
2.c Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C22(H22A,H22B,H22C)
;
_shelx_res_checksum              56187
_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
;