New homoleptic gold carbene complexes via Ag‒Au transmetalation: synthesis and application of [Au(diNHC)2]3+ cations as 1H-NMR and UV-vis halide sensors
Baron, Marco; Dall’Anese, Anna; Miolato, Alessandro; Cairoli, Maddalena L. C.; Di Marco, Valerio; Graiff, Claudia; Pöthig, Alexander; Tubaro, Cristina; New Journal of Chemistry 44 (2020) 5343–5353; doi:10.1039/C9NJ05809E

data_7059393
_publ_section_title
;
 New homoleptic gold carbene complexes via Ag--Au transmetalation:
 synthesis and application of [Au(diNHC)2]3+ cations as 1H-NMR and UV-vis
 halide sensors
;
_journal_issue                   14
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              5343
_journal_page_last               5353
_journal_paper_doi               10.1039/C9NJ05809E
_journal_volume                  44
_journal_year                    2020
_chemical_formula_moiety         '2(C10 H14 Au0.5 N4 O), 3(Cl), 2(C2 H6 O S)'
_chemical_formula_sum            'C24 H40 Au Cl3 N8 O4 S2'
_chemical_formula_weight         872.07
_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
_audit_creation_date             2019-11-07
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-11-11 deposited with the CCDC.	2020-03-10 downloaded from the CCDC.
;
_cell_angle_alpha                82.052(2)
_cell_angle_beta                 81.090(2)
_cell_angle_gamma                72.743(2)
_cell_formula_units_Z            2
_cell_length_a                   10.2116(7)
_cell_length_b                   11.6009(8)
_cell_length_c                   14.6925(10)
_cell_measurement_reflns_used    9674
_cell_measurement_temperature    101(2)
_cell_measurement_theta_max      28.31
_cell_measurement_theta_min      2.21
_cell_volume                     1634.24(19)
_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    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.91
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0282
_diffrn_reflns_av_unetI/netI     0.0114
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            124019
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.339
_diffrn_reflns_theta_min         2.377
_exptl_absorpt_coefficient_mu    4.918
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5354
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0741 before and 0.0423 after correction.
The Ratio of minimum to maximum transmission is 0.7180.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.772
_exptl_crystal_description       prism
_exptl_crystal_F_000             868
_exptl_crystal_size_max          0.358
_exptl_crystal_size_mid          0.166
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.498
_refine_diff_density_min         -1.599
_refine_diff_density_rms         0.089
_refine_ls_extinction_coef       0.00327(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/1 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     393
_refine_ls_number_reflns         8155
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0213
_refine_ls_R_factor_gt           0.0179
_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^)+(0.0085P)^2^+3.8541P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0386
_refine_ls_wR_factor_ref         0.0398
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7404
_reflns_number_total             8155
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nj05809e2.cif
_cod_data_source_block           '[au2l42](cl)3'
_cod_depositor_comments
;Adding full bibliography for 7059387--7059393.cif.

 Adding full bibliography for 7059387--7059393.cif.
;
_cod_original_cell_volume        1634.2(2)
_cod_database_code               7059393
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.614
_shelx_estimated_absorpt_t_min   0.272
_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, All O(H) groups
2.a Ternary CH refined with riding coordinates:
 C5(H5), C15(H15)
2.b Secondary CH2 refined with riding coordinates:
 C16(H16A,H16B), C6(H6A,H6B)
2.c Aromatic/amide H refined with riding coordinates:
 C9(H9), C8(H8), C19(H19), C3(H3), C18(H18), C4(H4), C13(H13), C14(H14)
2.d Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C2(H2A,H2B,H2C), C10(H10A,H10B,H10C), C20(H20A,H20B,
 H20C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C24(H24A,H24B,H24C), C23(H23A,
 H23B,H23C)
2.e Idealised tetrahedral OH refined as rotating group:
 O1(H1), O2(H2)
;
_shelx_res_checksum              56003
_olex2_submission_special_instructions 'No special instructions were received'