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_1569290
_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         'C56 H50 Au2 N6'
_chemical_formula_sum            'C56 H50 Au2 N6'
_chemical_formula_weight         1200.96
_chemical_name_systematic        XM487-2
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-03-04
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-10-18 deposited with the CCDC.	2023-06-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.3770(10)
_cell_angle_gamma                90
_cell_formula_units_Z            20
_cell_length_a                   27.2565(3)
_cell_length_b                   17.0998(2)
_cell_length_c                   52.0080(6)
_cell_measurement_reflns_used    44549
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.2860
_cell_measurement_theta_min      2.8060
_cell_volume                     23763.6(5)
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (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 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_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 0.871
_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    -37.00  63.50   0.75   20.00    --   -8.69  57.00 120.00  134
  2  \w    -82.00  18.50   0.75   20.00    --   -8.69 -57.00 -30.00  134
  3  \w    -20.00  80.50   0.75   20.00    --    7.83  57.00-150.00  134
  4  \w    -15.00  10.50   0.75   20.00    --    7.83 -99.00 -90.00   34
  5  \w      2.00  51.50   0.75   20.00    --    7.83-120.00  38.00   66
;
_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      0.0131455000
_diffrn_orient_matrix_UB_12      -0.0068373000
_diffrn_orient_matrix_UB_13      0.0129938000
_diffrn_orient_matrix_UB_21      0.0005420000
_diffrn_orient_matrix_UB_22      -0.0406244000
_diffrn_orient_matrix_UB_23      -0.0026737000
_diffrn_orient_matrix_UB_31      0.0230593000
_diffrn_orient_matrix_UB_32      0.0048285000
_diffrn_orient_matrix_UB_33      -0.0041848000
_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  0.0723
_diffrn_reflns_av_unetI/netI     0.0749
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.871
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       65
_diffrn_reflns_limit_l_min       -69
_diffrn_reflns_number            123620
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.871
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.763
_diffrn_reflns_theta_min         2.513
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    6.211
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.680
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
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            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.678
_exptl_crystal_description       irregular
_exptl_crystal_F_000             11720
_exptl_crystal_preparation       Synthesis
_exptl_crystal_recrystallization_method 'Hexane/DCM diffusion'
_exptl_crystal_size_max          0.217
_exptl_crystal_size_mid          0.114
_exptl_crystal_size_min          0.103
_refine_diff_density_max         2.006
_refine_diff_density_min         -1.374
_refine_diff_density_rms         0.191
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1457
_refine_ls_number_reflns         26919
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0842
_refine_ls_R_factor_gt           0.0583
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0079P)^2^+596.2996P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0932
_refine_ls_wR_factor_ref         0.1014
_reflns_Friedel_coverage         0.000
_reflns_number_gt                21244
_reflns_number_total             26919
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cy00716b2.cif
_cod_data_source_block           xm487-2
_cod_depositor_comments
'Adding full bibliography for 1569289--1569290.cif.'
_cod_database_code               1569290
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C56 H50 Au2 N6 '
_reflns_odcompleteness_completeness 99.87
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.07
_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:
 C25(H25A,H25B), C32(H32A,H32B), C81(H81A,H81B), C88(H88A,H88B), C137(H13J,H13K)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C8(H8), C9(H9), C10(H10), C11(H11), C14(H14),
 C15(H15), C18(H18), C20(H20), C27(H27), C29(H29), C30(H30), C31(H31), C34(H34),
  C35(H35), C38(H38), C40(H40), C46(H46), C47(H47), C48(H48), C49(H49),
 C52(H52), C53(H53), C54(H54), C55(H55), C58(H58), C59(H59), C60(H60), C61(H61),
  C64(H64), C65(H65), C66(H66), C67(H67), C70(H70), C71(H71), C74(H74),
 C76(H76), C83(H83), C85(H85), C86(H86), C87(H87), C90(H90), C91(H91), C94(H94),
  C96(H96), C102(H102), C103(H103), C104(H104), C105(H105), C108(H108),
 C109(H109), C110(H110), C111(H111), C114(H114), C115(H115), C116(H116),
 C117(H117), C120(H120), C121(H121), C122(H122), C123(H123), C126(H126),
 C127(H127), C130(H130), C132(H132), C139(H139), C140(H140), C141(H141)
2.c Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C42(H42A,H42B,
 H42C), C43(H43A,H43B,H43C), C44(H44A,H44B,H44C), C78(H78A,H78B,H78C), C79(H79A,
 H79B,H79C), C80(H80A,H80B,H80C), C98(H98A,H98B,H98C), C99(H99A,H99B,H99C),
 C100(H10A,H10B,H10C), C134(H13A,H13B,H13C), C135(H13D,H13E,H13F), C136(H13G,
 H13H,H13I)
;
_shelx_res_checksum              67004
_shelx_hkl_checksum              31891
_olex2_date_sample_data_collection 2022-03-03
_olex2_exptl_crystal_mounting_method 'Litho loop'
_olex2_submission_original_sample_id XM487-2
_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
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 1.405
_oxdiff_exptl_absorpt_empirical_full_min 0.799