Gold and Palladium Mediated Bimetallic Catalysis: Mechanistic Investigation through the Isolation of the Organogold(I) Intermediates
Verlee, Arno; Heugebaert, Thomas; van der Meer, Tom; Kerchev, Pavel; Van Hecke, Kristof; Van Breusegem, Frank; Stevens, Christian V.; ACS Catalysis 9 (2019) 7862–; doi:10.1021/acscatal.9b02275

data_4514817
_publ_section_title
;
 Gold and Palladium Mediated Bimetallic Catalysis: Mechanistic
 Investigation through the Isolation of the Organogold(I) Intermediates
;
_journal_issue                   9
_journal_name_full               'ACS Catalysis'
_journal_page_first              7862
_journal_paper_doi               10.1021/acscatal.9b02275
_journal_volume                  9
_journal_year                    2019
_chemical_formula_moiety         'C30 H25 Au N O2 P'
_chemical_formula_sum            'C30 H25 Au N O2 P'
_chemical_formula_weight         659.45
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2019-01-21
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 98.0363(14)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.35599(18)
_cell_length_b                   11.54410(18)
_cell_length_c                   17.5685(3)
_cell_measurement_reflns_used    16245
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      29.3730
_cell_measurement_theta_min      3.5080
_cell_volume                     2481.34(7)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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    'ShelXS (Sheldrick, 2008)'
_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 0.903
_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    -22.00  87.00   1.00   12.00    --   10.40  77.00 -30.00  109
  2  \w    -20.00  51.00   1.00   12.00    --   10.40 -99.00  30.00   71
  3  \w    -64.00  35.00   1.00   12.00    --   10.40 -38.00  30.00   99
  4  \w    -86.00 -38.00   1.00   12.00    --  -11.11 153.00 110.33   48
  5  \w    -66.00  20.00   1.00   12.00    --   10.40 -77.00-120.00   86
;
_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      0.0498909000
_diffrn_orient_matrix_UB_12      -0.0167795000
_diffrn_orient_matrix_UB_13      0.0222406000
_diffrn_orient_matrix_UB_21      0.0293582000
_diffrn_orient_matrix_UB_22      0.0235621000
_diffrn_orient_matrix_UB_23      -0.0283054000
_diffrn_orient_matrix_UB_31      0.0026737000
_diffrn_orient_matrix_UB_32      0.0542127000
_diffrn_orient_matrix_UB_33      0.0191768000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0540
_diffrn_reflns_av_unetI/netI     0.0455
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.903
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            26593
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.903
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.652
_diffrn_reflns_theta_min         2.590
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    6.022
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.607
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
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    1.765
_exptl_crystal_description       block
_exptl_crystal_F_000             1288
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.224
_exptl_crystal_size_min          0.133
_refine_diff_density_max         2.477
_refine_diff_density_min         -2.427
_refine_diff_density_rms         0.160
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         6336
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0354
_refine_ls_R_factor_gt           0.0299
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0323P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0651
_refine_ls_wR_factor_ref         0.0691
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5661
_reflns_number_total             6336
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs9b02275_si_003.cif
_cod_data_source_block           cs041
_cod_database_code               4514817
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C30 H25 Au N O2 P'
_shelx_estimated_absorpt_t_max   0.501
_shelx_estimated_absorpt_t_min   0.197
_reflns_odcompleteness_completeness 99.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B)
2.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C8(H8), C9(H9), C11(H11), C14(H14), C15(H15),
 C16(H16), C17(H17), C18(H18), C20(H20), C21(H21), C22(H22), C23(H23), C24(H24),
  C26(H26), C27(H27), C28(H28), C29(H29), C30(H30)
2.c X=CH2 refined with riding coordinates:
 C12(H12A,H12B)
;
_shelx_res_checksum              39196
_shelx_hkl_checksum              99538
_olex2_exptl_crystal_mounting_method 'mounted on a nylon loop'
_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 6.366
_oxdiff_exptl_absorpt_empirical_full_min 0.664