Synthesis and reactivity of N-heterocyclic carbene (NHC) gold-fluoroalkoxide complexes.
Arnaut, Pierre; Bracho Pozsoni, Nestor; Nahra, Fady; Tzouras, Nikolaos V.; Nolan, Steven P.; Dalton transactions (Cambridge, England : 2003) 53 (2024) 11952–11958; doi:10.1039/d4dt01402b

data_7716484
_publ_section_title
;
 Synthesis and reactivity of N-heterocyclic carbene (NHC)
 gold-fluoroalkoxide complexes.
;
_journal_issue                   28
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11952
_journal_page_last               11958
_journal_paper_doi               10.1039/d4dt01402b
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C40 H41 Au F6 N2 O'
_chemical_formula_sum            'C40 H41 Au F6 N2 O'
_chemical_formula_weight         876.71
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-10-02
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2023-12-01 deposited with the CCDC.	2024-06-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.739(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.3889(3)
_cell_length_b                   14.3510(5)
_cell_length_c                   23.1192(5)
_cell_measurement_reflns_used    16031
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      28.5650
_cell_measurement_theta_min      2.9380
_cell_volume                     3770.61(18)
_computing_cell_refinement       'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_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_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 0.901
_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    -42.00  43.00   1.00   17.50    --   10.01 -77.00 120.00   85
  2  \w     39.00  99.00   1.00   17.50    --   10.01 178.00-180.00   60
  3  \w    -18.00  83.00   1.00   17.50    --   10.01  57.00 -60.00  101
  4  \w    -42.00  21.00   1.00   17.50    --  -11.26 -77.00  30.00   63
  5  \w    -63.00 -26.00   1.00   17.50    --   10.01 -57.00 -30.00   37
  6  \w     37.00  97.00   1.00   17.50    --   10.01-178.00 -30.00   60
;
_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      -0.0036020000
_diffrn_orient_matrix_UB_12      0.0411527000
_diffrn_orient_matrix_UB_13      0.0167619000
_diffrn_orient_matrix_UB_21      -0.0231665000
_diffrn_orient_matrix_UB_22      -0.0262519000
_diffrn_orient_matrix_UB_23      0.0226629000
_diffrn_orient_matrix_UB_31      0.0578445000
_diffrn_orient_matrix_UB_32      -0.0077369000
_diffrn_orient_matrix_UB_33      0.0122774000
_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  0.0569
_diffrn_reflns_av_unetI/netI     0.0572
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.901
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            42903
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.901
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.646
_diffrn_reflns_theta_min         2.492
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.964
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76262
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.112a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.544
_exptl_crystal_description       plate
_exptl_crystal_F_000             1744
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.641
_refine_diff_density_min         -1.520
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     459
_refine_ls_number_reflns         9586
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0616
_refine_ls_R_factor_gt           0.0373
_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^)+(0.0218P)^2^+2.7940P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0630
_refine_ls_wR_factor_ref         0.0717
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7327
_reflns_number_total             9586
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01402b2.cif
_cod_data_source_block           pa167
_cod_depositor_comments          'Adding full bibliography for 7716484.cif.'
_cod_database_code               7716484
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C40H41Au1F6N2O1
_shelx_estimated_absorpt_t_max   0.890
_shelx_estimated_absorpt_t_min   0.570
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C10(H10), C13(H13), C32(H32), C35(H35), C38(H38)
2.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C17(H17), C18(H18), C19(H19), C21(H21), C22(H22),
 C23(H23), C28(H28), C29(H29), C30(H30)
2.c Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C15(H15A,H15B,
 H15C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C36(H36A,H36B,H36C), C37(H37A,
 H37B,H37C)
;
_shelx_res_checksum              76217
_shelx_hkl_checksum              5056
_olex2_date_sample_data_collection 2023-09-29
_olex2_exptl_crystal_mounting_method 'Mounted on a LythoLoop'
_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 1.338
_oxdiff_exptl_absorpt_empirical_full_min 0.791