Synthesis, conformational analysis and antibacterial activity of Au(I)-Ag(I) and Au(I)-Hg(II) heterobimetallic N-heterocyclic carbene complexes.
Li, Zili; Mackie, Emily R. R.; Ramkissoon, Pria; Mather, Joel C.; Wiratpruk, Nuchareenat; Soares da Costa, Tatiana P.; Barnard, Peter J.; Dalton transactions (Cambridge, England : 2003) 49 (2020) 12820–12834; doi:10.1039/d0dt02225j

data_7705335
_publ_section_title
;
 Synthesis, conformational analysis and antibacterial activity of
 Au(I)-Ag(I) and Au(I)-Hg(II) heterobimetallic N-heterocyclic carbene
 complexes.
;
_journal_issue                   36
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12820
_journal_page_last               12834
_journal_paper_doi               10.1039/d0dt02225j
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C9 H13 N4, I'
_chemical_formula_sum            'C9 H13 I N4'
_chemical_formula_weight         304.13
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2020-08-16
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-08-17 deposited with the CCDC.	2020-09-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 124.136(12)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.8428(6)
_cell_length_b                   11.5230(5)
_cell_length_c                   17.2878(15)
_cell_measurement_reflns_used    5123
_cell_measurement_temperature    133.0(4)
_cell_measurement_theta_max      76.5850
_cell_measurement_theta_min      4.9220
_cell_volume                     1128.3(2)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      133.0(4)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3309
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  70.00   1.00    1.00    --   41.58 -57.00   0.00   94
  2  \w     16.00  42.00   1.00    1.00    --   41.58 -77.00   0.00   26
  3  \w      2.00  95.00   1.00    1.00    --   41.58-125.00 -90.00   93
  4  \w     43.00  75.00   1.00    4.00    --  112.00 -61.00-120.00   32
  5  \w     89.00 115.00   1.00    4.00    --  112.00 -61.00-120.00   26
  6  \w     76.00 104.00   1.00    4.00    --  112.00-111.00 -60.00   28
  7  \w     89.00 116.00   1.00    4.00    --  112.00-111.00-150.00   27
  8  \w     41.00 115.00   1.00    4.00    --  112.00-111.00 -30.00   74
  9  \w     57.00 111.00   1.00    4.00    --  112.00-111.00  60.00   54
 10  \w     74.00 115.00   1.00    4.00    --  112.00-111.00 120.00   41
 11  \w     56.00 136.00   1.00    4.00    --  112.00 -45.00 120.00   80
 12  \w    122.00 148.00   1.00    4.00    --  112.00  15.00   0.00   26
 13  \w     79.00 130.00   1.00    4.00    --  112.00  77.00  90.00   51
 14  \w     95.00 121.00   1.00    4.00    --  112.00  61.00 150.00   26
 15  \w     65.00  96.00   1.00    4.00    --  112.00  15.00   0.00   31
 16  \w     36.00 127.00   1.00    4.00    --  112.00 -30.00 -90.00   91
 17  \w     92.00 158.00   1.00    4.00    --  112.00  45.00-180.00   66
 18  \w    113.00 155.00   1.00    4.00    --  112.00  61.00-150.00   42
 19  \w     81.00 157.00   1.00    4.00    --  112.00 111.00-150.00   76
 20  \w     63.00 128.00   1.00    4.00    --  112.00  15.00-180.00   65
 21  \w     36.00  62.00   1.00    4.00    --  112.00-111.00 -60.00   26
 22  \w     57.00  93.00   1.00    4.00    --  112.00-111.00  30.00   36
 23  \w     36.00  97.00   1.00    4.00    --  112.00-111.00  90.00   61
 24  \w     36.00 142.00   1.00    4.00    --  112.00 -77.00 120.00  106
 25  \w     28.00 116.00   1.00    1.00    --   41.58  38.00 150.00   88
 26  \w     22.00  58.00   1.00    1.00    --   41.58  57.00 -30.00   36
 27  \w    -33.00  -6.00   1.00    1.00    --   41.58 -77.00   0.00   27
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0382959000
_diffrn_orient_matrix_UB_12      0.1321592000
_diffrn_orient_matrix_UB_13      -0.0132979000
_diffrn_orient_matrix_UB_21      -0.0046491000
_diffrn_orient_matrix_UB_22      0.0069389000
_diffrn_orient_matrix_UB_23      0.0879630000
_diffrn_orient_matrix_UB_31      0.2692696000
_diffrn_orient_matrix_UB_32      0.0188473000
_diffrn_orient_matrix_UB_33      0.0606802000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0333
_diffrn_reflns_av_unetI/netI     0.0234
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            9269
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.480
_diffrn_reflns_theta_min         4.928
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    22.055
_exptl_absorpt_correction_T_max  0.98425
_exptl_absorpt_correction_T_min  0.98425
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Spherical absorption correction
 using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.790
_exptl_crystal_description       block
_exptl_crystal_F_000             592
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.626
_refine_diff_density_min         -1.334
_refine_diff_density_rms         0.136
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     128
_refine_ls_number_reflns         2314
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0324
_refine_ls_R_factor_gt           0.0296
_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^)+(0.0581P)^2^+0.8684P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0799
_refine_ls_wR_factor_ref         0.0842
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2138
_reflns_number_total             2314
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt02225j2.cif
_cod_data_source_block           10a
_cod_depositor_comments
;
Adding full bibliography for 7705334--7705337.cif.

2025-04-02
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C18 H26 I2 N8'
_cod_original_formula_weight         608.27
_cod_original_formula_moiety         '2(C9 H13 N4), 2(I)'
_cod_original_formula_units_Z            2
_cod_database_code               7705335
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C20 H20 N12 Br2'
_shelx_estimated_absorpt_t_max   0.667
_shelx_estimated_absorpt_t_min   0.472
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_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:
 C7(H7A,H7B), C8(H8A,H8B)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C6(H6)
2.c Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C)
;
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a mylar loop in perfluoroether oil'
_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 1.939
_oxdiff_exptl_absorpt_empirical_full_min 0.692