Novel dinuclear NHC–gold(i)-amido complexes and their application in energy transfer photocatalysis
Ma, Xinyuan; Voloshkin, Vladislav A.; Martynova, Ekaterina A.; Beliš, Marek; Peng, Min; Villa, Marco; Tzouras, Nikolaos V.; Janssens, Wim; Van Hecke, Kristof; Ceroni, Paola; Nolan, Steven P.; Catalysis Science & Technology 13 (2023) 4168–4175; doi:10.1039/D3CY00716B

data_1569289
_publ_section_title
;
 Novel dinuclear NHC--gold(i)-amido complexes and their application in
 energy transfer photocatalysis
;
_journal_issue                   14
_journal_name_full               'Catalysis Science &amp; Technology'
_journal_page_first              4168
_journal_page_last               4175
_journal_paper_doi               10.1039/D3CY00716B
_journal_volume                  13
_journal_year                    2023
_chemical_formula_moiety         'C62 H62 Au2 N6, 1[C4H8O]'
_chemical_formula_sum            'C66 H70 Au2 N6 O'
_chemical_formula_weight         1357.21
_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_creation_date             2022-03-25
_audit_creation_method
;
Olex2 1.5
(compiled 2021.08.20 svn.r13c46975 for OlexSys, GUI svn.r6396)
;
_audit_update_record
;
2022-10-18 deposited with the CCDC.	2023-06-19 downloaded from the CCDC.
;
_cell_angle_alpha                103.775(2)
_cell_angle_beta                 95.912(2)
_cell_angle_gamma                101.539(2)
_cell_formula_units_Z            2
_cell_length_a                   12.4705(2)
_cell_length_b                   14.3086(3)
_cell_length_c                   17.1528(3)
_cell_measurement_reflns_used    18849
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      73.7870
_cell_measurement_theta_min      2.6480
_cell_volume                     2875.84(10)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_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_environment      N~2~
_diffrn_ambient_temperature      100.0(1)
_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 0.980
_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   -116.00 -17.00   1.00    1.00    --  -41.55 -38.00  90.00   99
  2  \w    -66.00  33.00   1.00    1.00    --  -41.55  38.00 -90.00   99
  3  \w    -38.00  83.00   1.00    1.00    --   41.55 -19.00 -60.00  121
  4  \w     27.00  98.00   1.00    1.00    --   41.55-125.00  60.00   71
  5  \w      6.00  82.00   1.00    1.00    --   41.55 -99.00-120.00   76
  6  \w     33.00 112.00   1.00    1.75    --  106.01-125.00 -30.00   79
  7  \w     23.00 107.00   1.00    1.75    --  106.01 -94.00  90.00   84
  8  \w     77.00 178.00   1.00    1.75    --  106.01  61.00-120.00  101
  9  \w    103.00 178.00   1.00    1.75    --  106.01  77.00-180.00   75
 10  \w     33.00 132.00   1.00    1.75    --  106.01 -45.00  90.00   99
 11  \w     53.00 178.00   1.00    1.75    --  106.01  15.00   0.00  125
 12  \w     34.00 135.00   1.00    1.75    --  106.01 -61.00-150.00  101
 13  \w     77.00 178.00   1.00    1.75    --  106.01  61.00  30.00  101
 14  \w     23.00 107.00   1.00    1.75    --  106.01 -94.00   0.00   84
 15  \w     23.00 107.00   1.00    1.75    --  106.01 -94.00-180.00   84
 16  \w   -114.00 -13.00   1.00    1.00    --  -41.55 -57.00-150.00  101
 17  \w    -87.00  -6.00   1.00    1.00    --  -41.55 125.00  60.00   81
 18  \w   -114.00 -13.00   1.00    1.00    --  -41.55 -57.00 -60.00  101
 19  \w   -114.00 -13.00   1.00    1.00    --  -41.55 -57.00  30.00  101
 20  \w     13.00 114.00   1.00    1.00    --   41.55  57.00-150.00  101
 21  \w     80.00 178.00   1.00    1.75    --  106.01  45.00-180.00   98
 22  \w     77.00 178.00   1.00    1.75    --  106.01  61.00 -30.00  101
 23  \w     78.00 178.00   1.00    1.75    --  106.01  30.00 120.00  100
 24  \w     77.00 178.00   1.00    1.75    --  106.01  61.00   0.00  101
 25  \w     77.00 128.00   1.00    1.75    --  106.01  61.00-150.00   51
 26  \w     87.00 101.00   1.00    1.75    --  106.01  61.00  60.00   14
 27  \w    110.00 122.00   1.00    1.75    --  106.01  61.00 -90.00   12
 28  \w     80.00 178.00   1.00    1.75    --  106.01  45.00 120.00   98
 29  \w     77.00 178.00   1.00    1.75    --  106.01  61.00 -60.00  101
 30  \w     80.00 178.00   1.00    1.75    --  106.01  45.00 150.00   98
 31  \w   -114.00 -13.00   1.00    1.00    --  -41.55 -57.00 -30.00  101
;
_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      -0.0370899000
_diffrn_orient_matrix_UB_12      -0.1063684000
_diffrn_orient_matrix_UB_13      -0.0554488000
_diffrn_orient_matrix_UB_21      0.0241896000
_diffrn_orient_matrix_UB_22      0.0389710000
_diffrn_orient_matrix_UB_23      -0.0742355000
_diffrn_orient_matrix_UB_31      0.1197710000
_diffrn_orient_matrix_UB_32      -0.0125635000
_diffrn_orient_matrix_UB_33      0.0136272000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0631
_diffrn_reflns_av_unetI/netI     0.0515
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            49365
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.860
_diffrn_reflns_theta_min         2.686
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.814
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.440
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.567
_exptl_crystal_description       block
_exptl_crystal_F_000             1348
_exptl_crystal_preparation       synthesis
_exptl_crystal_size_max          0.57
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.058
_refine_diff_density_min         -1.169
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     639
_refine_ls_number_reflns         11431
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.0574
_refine_ls_R_factor_gt           0.0391
_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^)+(0.0347P)^2^+4.6589P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0823
_refine_ls_wR_factor_ref         0.0892
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8722
_reflns_number_total             11431
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cy00716b2.cif
_cod_data_source_block           xm_483_a_2
_cod_depositor_comments
'Adding full bibliography for 1569289--1569290.cif.'
_cod_database_code               1569289
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C66 H70 Au2 N6 O'
_shelx_estimated_absorpt_t_max   0.757
_shelx_estimated_absorpt_t_min   0.071
_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 Ternary CH refined with riding coordinates:
 C22(H22), C25(H25), C45(H45), C48(H48)
2.b Secondary CH2 refined with riding coordinates:
 C28(H28A,H28B), C35(H35A,H35B)
2.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11), C14(H14),
 C15(H15), C16(H16), C17(H17), C21(H21), C29(H29), C30(H30), C32(H32), C33(H33),
  C36(H36), C37(H37), C41(H41), C42(H42), C43(H43), C52(H52), C53(H53),
 C54(H54), C55(H55), C59(H59), C60(H60), C61(H61), C62(H62)
2.d Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C27(H27A,H27B,
 H27C), C46(H46A,H46B,H46C), C47(H47A,H47B,H47C), C49(H49A,H49B,H49C), C50(H50A,
 H50B,H50C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 40 electrons were 
found in a volume of 170\%A^3^ in 2 voids per Assymetric 
Unit. This is consistent with the presence of 
1[C4H8O] per Asymmetric Unit 
which account for 80 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              25072
_shelx_hkl_checksum              75719
_shelx_fab_checksum              59173
_olex2_date_sample_data_collection 2022-03-04
_olex2_exptl_crystal_mounting_method 'Mounted on a LithoLoop'
_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 1.396
_oxdiff_exptl_absorpt_empirical_full_min 0.690