Synthesis of a (N,C,C) Au(iii) pincer complex via C<sub>sp<sup>3</sup></sub>-H bond activation: increasing catalyst robustness by rational catalyst design.
Holmsen, Marte Sofie Martinsen; Nova, Ainara; Hylland, Knut; Wragg, David S.; Øien-Ødegaard, Sigurd; Heyn, Richard H.; Tilset, Mats; Chemical communications (Cambridge, England) 54 (2018) 11104–11107; doi:10.1039/c8cc05489d

data_7122318
_publ_section_title
;
 Synthesis of a (N,C,C) Au(iii) pincer complex via
 C<sub>sp<sup>3</sup></sub>-H bond activation: increasing catalyst
 robustness by rational catalyst design.
;
_journal_issue                   79
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              11104
_journal_page_last               11107
_journal_paper_doi               10.1039/c8cc05489d
_journal_volume                  54
_journal_year                    2018
_chemical_formula_moiety         'C21 H23 Au F3 N O2'
_chemical_formula_sum            'C21 H23 Au F3 N O2'
_chemical_formula_weight         575.37
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-08-17
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-08-17 deposited with the CCDC.
2018-09-06 downloaded from the CCDC.
;
_cell_angle_alpha                94.949(2)
_cell_angle_beta                 95.354(2)
_cell_angle_gamma                104.902(2)
_cell_formula_units_Z            2
_cell_length_a                   8.7448(5)
_cell_length_b                   9.6069(6)
_cell_length_c                   12.4327(7)
_cell_measurement_reflns_used    9993
_cell_measurement_temperature    105(2)
_cell_measurement_theta_max      32.136
_cell_measurement_theta_min      2.604
_cell_volume                     998.32(10)
_computing_cell_refinement       'APEX3 (Bruker AXS, 2016)'
_computing_data_collection       'APEX3 (Bruker AXS, 2016)'
_computing_data_reduction        'APEX3 (Bruker AXS, 2016)'
_computing_molecular_graphics    'Diamond v4 (Brandenburg, 2012)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015b)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015a)'
_diffrn_ambient_temperature      105.15
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker D8 Venture, CMOS detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0457
_diffrn_reflns_av_unetI/netI     0.0389
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            26763
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.177
_diffrn_reflns_theta_min         2.208
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.411
_exptl_absorpt_correction_T_max  0.7463
_exptl_absorpt_correction_T_min  0.1599
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1755 before and 0.0840 after correction. The Ratio of minimum to maximum transmission is 0.2143. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.914
_exptl_crystal_description       block
_exptl_crystal_F_000             556
_exptl_crystal_size_max          1
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.21
_refine_diff_density_max         1.662
_refine_diff_density_min         -2.865
_refine_diff_density_rms         0.229
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     258
_refine_ls_number_reflns         6990
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0398
_refine_ls_R_factor_gt           0.0326
_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^)+(0.0391P)^2^+3.1444P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0777
_refine_ls_wR_factor_ref         0.0808
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6325
_reflns_number_total             6990
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc05489d2.cif
_cod_data_source_block           msh-699-soe_pl
_cod_depositor_comments          'Adding full bibliography for 7122318.cif.'
_cod_database_code               7122318
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.305
_shelx_estimated_absorpt_t_min   0.051
_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:
 C8(H8A,H8B)
2.b Aromatic/amide H refined with riding coordinates:
 C19(H19), C20(H20), C21(H21), C18(H18), C13(H13), C11(H11)
2.c Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C15(H15A,H15B,H15C), C16(H16A,H16B,
 H16C), C17(H17A,H17B,H17C)
;
_olex2_submission_special_instructions 'No special instructions were received'