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_7710763
_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         'C20 H20 Ag2 Cl2 N4'
_chemical_formula_sum            'C20 H20 Ag2 Cl2 N4'
_chemical_formula_weight         603.04
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2021-07-26
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2022-05-19 deposited with the CCDC.	2022-07-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.300(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.2662(2)
_cell_length_b                   7.39800(10)
_cell_length_c                   12.5768(2)
_cell_measurement_reflns_used    14850
_cell_measurement_temperature    150(15)
_cell_measurement_theta_max      27.2930
_cell_measurement_theta_min      3.2910
_cell_volume                     1041.91(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 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(15)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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     -8.00  47.00   0.50   10.00    --    9.52-107.00 -37.00  110
  2  \w    -27.00  54.00   0.50   10.00    --   -9.44  57.00   0.00  162
  3  \w    -80.00   3.00   0.50   10.00    --   -9.44 -19.00-120.00  166
  4  \w      1.00  35.00   0.50   10.00    --   -9.44-118.00 156.09   68
  5  \w      4.00  36.00   0.50   10.00    --   -9.44-121.00  52.37   64
  6  \w    -73.00   4.00   0.50   10.00    --   -9.44 -38.00  60.00  154
  7  \w    -80.00   3.00   0.50   10.00    --   -9.44 -19.00 150.00  166
  8  \w      6.00  38.00   0.50   10.00    --   -9.44-124.00 -27.64   64
  9  \w    -35.00  20.00   0.50   10.00    --   -9.44  77.00   0.00  110
 10  \w    -21.00  61.00   0.50   10.00    --   -9.44  19.00  90.00  164
 11  \w    -27.00  54.00   0.50   10.00    --   -9.44  57.00 150.00  162
 12  \w      2.00  35.00   0.50   10.00    --   -9.44-119.00  98.24   66
 13  \w      7.00  58.00   0.50   10.00    --    9.52-125.00  90.00  102
 14  \w     10.00  62.00   0.50   10.00    --    9.52-131.00-120.02  104
 15  \w      7.00  58.00   0.50   10.00    --    9.52-125.00 120.00  102
 16  \w      7.00  58.00   0.50   10.00    --    9.52-125.00 -60.00  102
 17  \w      7.00  58.00   0.50   10.00    --    9.52-125.00-180.00  102
 18  \w      7.00  58.00   0.50   10.00    --    9.52-125.00 -90.00  102
 19  \w      7.00  58.00   0.50   10.00    --    9.52-125.00 -30.00  102
 20  \w    -54.00  23.00   0.50   10.00    --    9.52 -38.00-120.00  154
 21  \w    -41.00   8.00   0.50   10.00    --   -9.44 -77.00-120.00   98
 22  \w    -73.00   4.00   0.50   10.00    --   -9.44 -38.00 -30.00  154
;
_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           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0731
_diffrn_reflns_av_unetI/netI     0.0449
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            21372
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        24.703
_diffrn_reflns_theta_max         24.703
_diffrn_reflns_theta_min         3.200
_exptl_absorpt_coefficient_mu    2.149
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72878
_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    1.922
_exptl_crystal_description       block
_exptl_crystal_F_000             592
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.372
_refine_diff_density_min         -0.341
_refine_diff_density_rms         0.080
_refine_ls_abs_structure_details
;
 Flack x determined using 1441 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.01(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     255
_refine_ls_number_reflns         3544
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0300
_refine_ls_R_factor_gt           0.0275
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0255P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0580
_refine_ls_wR_factor_ref         0.0598
_reflns_Friedel_coverage         0.841
_reflns_Friedel_fraction_full    0.996
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                3358
_reflns_number_total             3544
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01657e2.cif
_cod_data_source_block           3a
_cod_database_code               7710763
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.919
_shelx_estimated_absorpt_t_min   0.847
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C17(H17), C9(H9), C16(H16), C7(H7), C18(H18), C19(H19), C15(H15), C3(H3),
 C2(H2), C6(H6), C8(H8), C5(H5), C12(H12), C13(H13)
2.b Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C10(H10A,H10B,H10C)
;
_shelx_res_checksum              80398
_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
;