Dinuclear NHC-gold(I)-thiolato and -alkynyl complexes: synthesis, anticancer activity, and catalytic activity in lactonization reactions.
Ma, Xinyuan; Zhao, Yuan; Caligiuri, Isabella; Rizzolio, Flavio; Bracho Pozsoni, Nestor; Van Hecke, Kristof; Scattolin, Thomas; Nolan, Steven P.; Dalton transactions (Cambridge, England : 2003) 53 (2024) 7939–7945; doi:10.1039/d4dt00890a

data_7715755
_publ_section_title
;
 Dinuclear NHC-gold(I)-thiolato and -alkynyl complexes: synthesis,
 anticancer activity, and catalytic activity in lactonization reactions.
;
_journal_issue                   18
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7939
_journal_page_last               7945
_journal_paper_doi               10.1039/d4dt00890a
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C50 H56 Au2 N4 S2'
_chemical_formula_sum            'C50 H56 Au2 N4 S2'
_chemical_formula_weight         1171.04
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc2jl1t0
_audit_creation_date             2024-03-15
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-03-18 deposited with the CCDC.	2024-04-17 downloaded from the CCDC.
;
_cell_angle_alpha                110.305(2)
_cell_angle_beta                 101.236(2)
_cell_angle_gamma                92.613(2)
_cell_formula_units_Z            2
_cell_length_a                   9.7037(2)
_cell_length_b                   14.9460(4)
_cell_length_c                   16.9881(5)
_cell_measurement_reflns_used    16189
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.4230
_cell_measurement_theta_min      2.7450
_cell_volume                     2249.19(11)
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (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 2018/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4839
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.878
_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    -67.00  32.00   1.00    3.00    --    7.68 -38.00  90.00   99
  2  \w    -17.00  82.00   1.00    3.00    --    7.68  38.00 -90.00   99
  3  \w    -42.00  40.00   1.00    3.00    --    7.68 -77.00 -30.00   82
  4  \w    -42.00  24.00   1.00    3.00    --   -8.85 -77.00 -30.00   66
  5  \w    -17.00  82.00   1.00    3.00    --    7.68  38.00 150.00   99
  6  \w    -25.00  11.00   1.00    3.00    --    7.68  77.00   0.00   36
  7  \w    -67.00  32.00   1.00    3.00    --    7.68 -38.00 150.00   99
  8  \w    -41.00  21.00   1.00    3.00    --   -8.85  77.00  30.00   62
  9  \w    -41.00  21.00   1.00    3.00    --   -8.85  77.00-150.00   62
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0032266000
_diffrn_orient_matrix_UB_12      -0.0485690000
_diffrn_orient_matrix_UB_13      -0.0275086000
_diffrn_orient_matrix_UB_21      0.0418385000
_diffrn_orient_matrix_UB_22      -0.0100686000
_diffrn_orient_matrix_UB_23      0.0343986000
_diffrn_orient_matrix_UB_31      -0.0622767000
_diffrn_orient_matrix_UB_32      -0.0118149000
_diffrn_orient_matrix_UB_33      0.0121461000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0727
_diffrn_reflns_av_unetI/netI     0.0691
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.878
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            44349
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.878
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.761
_diffrn_reflns_theta_min         2.574
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    6.647
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.416
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dull light colourless'
_exptl_crystal_colour_lustre     dull
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.729
_exptl_crystal_description       plate
_exptl_crystal_F_000             1148
_exptl_crystal_recrystallization_method 'Dichloromethane and Pentane'
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.07
_refine_diff_density_max         2.004
_refine_diff_density_min         -1.433
_refine_diff_density_rms         0.197
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     531
_refine_ls_number_reflns         10251
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0592
_refine_ls_R_factor_gt           0.0384
_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^)+(0.0227P)^2^+3.2220P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0683
_refine_ls_wR_factor_ref         0.0767
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8020
_reflns_number_total             10251
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00890a2.cif
_cod_data_source_block           xmyz01
_cod_depositor_comments          'Adding full bibliography for 7715755.cif.'
_cod_database_code               7715755
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         'C1 H1 N1 Au1 S1'
_shelx_estimated_absorpt_t_max   0.653
_shelx_estimated_absorpt_t_min   0.204
_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. Uiso/Uaniso restraints and constraints
Uanis(C32) \\sim Ueq: with sigma of 0.003 and sigma for terminal atoms of 0.006
3.a Ternary CH refined with riding coordinates:
 C21(H21), C24(H24), C34(H34), C36(H36)
3.b Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C14(H14A,H14B)
3.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C9(H9), C10(H10), C11(H11), C12(H12),
 C17(H17), C18(H18), C19(H19), C29(H29), C30(H30), C31(H31), C40(H40), C41(H41),
  C42(H42), C43(H43), C44(H44), C46(H46), C47(H47), C48(H48), C49(H49), C50(H50)
3.d Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C25(H25A,H25B,H25C), C26(H26A,H26B,
 H26C), C33(H33A,H33B,H33C), C35(H35A,H35B,H35C), C37(H37A,H37B,H37C), C38(H38A,
 H38B,H38C)
;
_shelx_res_checksum              47204
_olex2_date_sample_data_collection 2024-01-26
_olex2_exptl_crystal_mounting_method 'Mounted on a Litholoop'
_olex2_submission_original_sample_id XMYZ01
_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 2.680
_oxdiff_exptl_absorpt_empirical_full_min 0.549