Energy transfer (EnT) photocatalysis enabled by Gold-N-heterocyclic carbene (NHC) complexes
Martynova, Ekaterina A.; Voloshkin, Vladislav; Guillet, Sébastien; Bru, Francis; Belis, Marek; Van Hecke, Kristof; Cazin, Catherine; Nolan, Steven P.; Chemical Science  (2022) –; doi:10.1039/D2SC00864E

data_1566995
_publ_section_title
;
 Energy transfer (EnT) photocatalysis enabled by Gold-N-heterocyclic
 carbene (NHC) complexes
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D2SC00864E
_journal_year                    2022
_chemical_formula_moiety         'C22 H27 N O5'
_chemical_formula_sum            'C22 H27 N O5'
_chemical_formula_weight         385.45
_chemical_name_systematic        VL575
_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     iterative
_audit_creation_date             2022-01-27
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-02-02 deposited with the CCDC.	2022-05-18 downloaded from the CCDC.
;
_cell_angle_alpha                84.544(2)
_cell_angle_beta                 81.654(3)
_cell_angle_gamma                83.321(3)
_cell_formula_units_Z            2
_cell_length_a                   7.4056(2)
_cell_length_b                   9.4530(3)
_cell_length_c                   15.2930(5)
_cell_measurement_reflns_used    9058
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      73.6590
_cell_measurement_theta_min      2.9080
_cell_volume                     1048.73(6)
_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    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.4839
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.981
_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    -70.00  31.00   1.00    1.00    --  -41.68  57.00 -60.00  101
  2  \w   -115.00 -14.00   1.00    1.00    --  -41.68 -57.00 150.00  101
  3  \w     27.00  98.00   1.00    1.00    --   41.68-125.00-180.00   71
  4  \w    -21.00  74.00   1.00    1.00    --   41.68 -77.00  30.00   95
  5  \w     23.00 107.00   1.00    2.00    --  106.01 -94.00  60.00   84
  6  \w     28.00 108.00   1.00    2.00    --  106.01-107.00-112.00   80
  7  \w     97.00 178.00   1.00    2.00    --  106.01 125.00 -60.00   81
  8  \w    103.00 178.00   1.00    2.00    --  106.01  77.00  90.00   75
  9  \w    103.00 178.00   1.00    2.00    --  106.01  77.00   0.00   75
 10  \w     23.00 107.00   1.00    2.00    --  106.01 -94.00 120.00   84
 11  \w     33.00 132.00   1.00    2.00    --  106.01 -45.00 -60.00   99
 12  \w     97.00 178.00   1.00    2.00    --  106.01 125.00  30.00   81
 13  \w     80.00 178.00   1.00    2.00    --  106.01  45.00 150.00   98
 14  \w     80.00 178.00   1.00    2.00    --  106.01  45.00-120.00   98
 15  \w     23.00 107.00   1.00    2.00    --  106.01 -94.00 -30.00   84
 16  \w   -115.00 -14.00   1.00    1.00    --  -41.68 -57.00  60.00  101
 17  \w    -66.00  33.00   1.00    1.00    --  -41.68  38.00-150.00   99
 18  \w   -115.00 -14.00   1.00    1.00    --  -41.68 -57.00 -30.00  101
 19  \w   -115.00 -14.00   1.00    1.00    --  -41.68 -57.00-120.00  101
 20  \w     77.00 178.00   1.00    2.00    --  106.01  61.00  30.00  101
 21  \w     77.00 178.00   1.00    2.00    --  106.01  61.00-180.00  101
 22  \w     53.00 178.00   1.00    2.00    --  106.01  15.00  60.00  125
 23  \w     77.00 178.00   1.00    2.00    --  106.01  61.00  60.00  101
 24  \w     80.00 178.00   1.00    2.00    --  106.01  45.00 -60.00   98
 25  \w     77.00 178.00   1.00    2.00    --  106.01  61.00 -90.00  101
 26  \w     80.00 178.00   1.00    2.00    --  106.01  45.00 -30.00   98
 27  \w     77.00 178.00   1.00    2.00    --  106.01  61.00  90.00  101
 28  \w   -115.00 -14.00   1.00    1.00    --  -41.68 -57.00 -90.00  101
 29  \w   -115.00 -14.00   1.00    1.00    --  -41.68 -57.00-150.00  101
 30  \w   -116.00 -17.00   1.00    1.00    --  -41.68 -38.00 -30.00   99
 31  \w     14.00 115.00   1.00    1.00    --   41.68  57.00 150.00  101
 32  \w     77.00 159.00   1.00    2.00    --  106.01  61.00   0.00   82
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0199
_diffrn_reflns_av_unetI/netI     0.0126
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            19741
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.926
_diffrn_reflns_theta_min         2.930
_exptl_absorpt_coefficient_mu    0.703
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.315
_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    1.221
_exptl_crystal_description       irregular
_exptl_crystal_F_000             412
_exptl_crystal_preparation       Synthesis
_exptl_crystal_recrystallization_method 'Hexane diffusion in CDCl3'
_exptl_crystal_size_max          0.356
_exptl_crystal_size_mid          0.281
_exptl_crystal_size_min          0.207
_refine_diff_density_max         0.296
_refine_diff_density_min         -0.289
_refine_diff_density_rms         0.039
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     265
_refine_ls_number_reflns         4169
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0678
_refine_ls_R_factor_gt           0.0596
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0935P)^2^+0.2368P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1717
_refine_ls_wR_factor_ref         0.1810
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3463
_reflns_number_total             4169
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc00864e2.cif
_cod_data_source_block           vl575
_cod_database_code               1566995
_shelx_shelxl_version_number     2018/3
_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. Restrained distances
 C18-C19
 1.51 with sigma of 0.003
 O5-C21B
 1.457 with sigma of 0.01
 O5-C21A
 1.457 with sigma of 0.01
 C22B-C21B = C21A-C22A
 1.491 with sigma of 0.01
 C20-C21A = C20-C21B
 2.373 with sigma of 0.02
 O5-C22A = O5-C22B
 2.376 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C21A) = Uanis(C21B)
Uanis(C22A) = Uanis(C22B)
4. Others
 Sof(C21A)=Sof(H21C)=Sof(H21D)=Sof(C22A)=Sof(H22D)=Sof(H22E)=Sof(H22F)=1-FVAR(1)
 Sof(C21B)=Sof(H21A)=Sof(H21B)=Sof(C22B)=Sof(H22A)=Sof(H22B)=Sof(H22C)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C8(H8)
5.b Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C11(H11A,H11B), C13(H13A,H13B), C18(H18A,H18B), C21B(H21A,H21B),
 C21A(H21C,H21D)
5.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5)
5.d Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C19(H19A,H19B,H19C), C22B(H22A,H22B,
 H22C), C22A(H22D,H22E,H22F)
;
_shelx_res_checksum              37301
_shelx_hkl_checksum              39561
_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
;