Gold(I) Catalyzes the Intermolecular Hydroamination of Alkynes with Imines and Produces α,α',N-Triarylbisenamines: Studies on Their Use As Intermediates in Synthesis
Antonio Leyva-Pérez; Jose R. Cabrero-Antonino; Ángel Cantín; Avelino Corma; Journal of Organic Chemistry 75 (2010) 7769–7780; doi:10.1021/jo101674t

data_4025834
_publ_contact_author_address
;
Instituto de Tecnolog\'ia Qu\'imica, 
Universidad Polit\'ecnica de Valencia-Consejo
Superior de Investigaciones Cient\'ificas. Avda. de los Naranjos s/n, 46022,
Valencia, Spain.
;
_publ_contact_author_email       anleyva@itq.upv.es
_publ_contact_author_name        'Leyva-P\'erez, Antonio'
_publ_section_title
;
 Gold(I) Catalyzes the Intermolecular Hydroamination of Alkynes with
 Imines and Produces \a,\a',N-Triarylbisenamines: Studies on Their Use As
 Intermediates in Synthesis
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              7769
_journal_page_last               7780
_journal_paper_doi               10.1021/jo101674t
_journal_volume                  75
_journal_year                    2010
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C29 H27 N1 O4'
_chemical_formula_sum            'C29 H27 N O4'
_chemical_formula_weight         453.52
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_creation_date             2010-03-04T12:49:56-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
?

2010-07-13 # Formatted by publCIF
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   7.5332(12)
_cell_length_b                   18.566(3)
_cell_length_c                   33.103(5)
_cell_measurement_reflns_used    1984
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      18.43
_cell_measurement_theta_min      2.19
_cell_measurement_wavelength     0.71073
_cell_volume                     4629.8(13)
_computing_cell_refinement       'APPEX2 (BRUKER AXS, 2005)'
_computing_data_collection       'APPEX2 (BRUKER AXS, 2005)'
_computing_data_reduction        'APPEX2 (BRUKER AXS, 2005)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR-97  (Giacovazzo et all, 1999)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'BRUKER APPEX-II CCD'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.2102
_diffrn_reflns_av_unetI/netI     0.1051
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            64702
_diffrn_reflns_theta_full        23.25
_diffrn_reflns_theta_max         23.25
_diffrn_reflns_theta_min         2.19
_exptl_absorpt_coefficient_mu    0.086
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.7072
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'BRUKER SADABS'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.301
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1920
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.296
_refine_diff_density_min         -0.279
_refine_diff_density_rms         0.073
_refine_ls_extinction_coef       0.0048(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     311
_refine_ls_number_reflns         3335
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.1325
_refine_ls_R_factor_gt           0.0652
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0826P)^2^+0.4631P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1312
_refine_ls_wR_factor_ref         0.1698
_reflns_number_gt                1936
_reflns_number_total             3335
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            jo101674t_si_005.cif
_cod_data_source_block           cc02zga1n
_cod_database_code               4025834