Catalytic domino amination and oxidative coupling of gold acetylides and isolation of key vinylene digold intermediates as a new class of ditopic N-heterocyclic carbene complexes
Zhang, Jun; Chen, Haifeng; Wang, Jiwei; Hu, Zejun; Xu, Sheng; Shi, Min; Chem. Commun.  (2017) –; doi:10.1039/C7CC06069F

data_7120640
_publ_section_title
;
 Catalytic domino amination and oxidative coupling of gold acetylides and
 isolation of key vinylene digold intermediates as a new class of ditopic
 N-heterocyclic carbene complexes
;
_journal_name_full               'Chem. Commun.'
_journal_paper_doi               10.1039/C7CC06069F
_journal_year                    2017
_chemical_formula_sum            'C36 H55 Au2 Cl2 N3 O'
_chemical_formula_weight         1010.66
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2015-12-02 deposited with the CCDC.
2017-09-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.7762(14)
_cell_length_b                   17.0556(19)
_cell_length_c                   18.581(2)
_cell_measurement_reflns_used    8215
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      23.24
_cell_measurement_theta_min      2.27
_cell_volume                     4048.9(8)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0487
_diffrn_reflns_av_unetI/netI     0.0489
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            35920
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.612
_diffrn_reflns_theta_min         1.934
_exptl_absorpt_coefficient_mu    7.399
_exptl_absorpt_correction_T_max  0.745
_exptl_absorpt_correction_T_min  0.598
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.658
_exptl_crystal_description       block
_exptl_crystal_F_000             1968
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.070
_refine_diff_density_max         0.512
_refine_diff_density_min         -0.577
_refine_diff_density_rms         0.097
_refine_ls_abs_structure_details
; 
 Flack x determined using 2932 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons and Flack (2004), Acta Cryst. A60, s61). 
;
_refine_ls_abs_structure_Flack   -0.006(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.998
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     416
_refine_ls_number_reflns         8474
_refine_ls_number_restraints     26
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.0395
_refine_ls_R_factor_gt           0.0264
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; 
 w=1/[\s^2^(Fo^2^)+(0.0116P)^2^] 
 where P=(Fo^2^+2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0479
_refine_ls_wR_factor_ref         0.0514
_reflns_Friedel_coverage         0.801
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                7222
_reflns_number_total             8474
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc06069f2.cif
_cod_data_source_block           mo_51016b
_cod_database_code               7120640
_shelx_estimated_absorpt_t_min   0.349
_shelx_estimated_absorpt_t_max   0.625
_shelxl_version_number           2013-2
_shelx_res_checksum              16649