Efficient Cycloisomerization of Propargyl Amides by Electrophilic Gold(I) Complexes of KITPHOS Monophosphines: A Comparative Study
Doherty, Simon; Knight, Julian G.; Hashmi, A. Stephen K.; Smyth, Catherine H.; Ward, Nicholas A. B.; Robson, Katharine J.; Tweedley, Sophie; Harrington, Ross W.; Clegg, William; Organometallics 29 (2010) 4139–; doi:10.1021/om1006769

data_4066844
_publ_section_title
;
 Efficient Cycloisomerization of Propargyl Amides by Electrophilic Gold(I)
 Complexes of KITPHOS Monophosphines: A Comparative Study
;
_journal_issue                   18
_journal_name_full               Organometallics
_journal_page_first              4139
_journal_paper_doi               10.1021/om1006769
_journal_volume                  29
_journal_year                    2010
_chemical_formula_moiety         'C36 H39 Au F3 O4 P S'
_chemical_formula_sum            'C36 H39 Au F3 O4 P S'
_chemical_formula_weight         852.67
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 96.282(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   20.9477(4)
_cell_length_b                   19.3370(3)
_cell_length_c                   16.9133(2)
_cell_measurement_reflns_used    18352
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.51
_cell_measurement_theta_min      2.87
_cell_volume                     6809.86(19)
_computing_cell_refinement       CrysAlisPro
_computing_data_collection       CrysAlisPro
_computing_data_reduction        CrysAlisPro
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL and local programs'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 10.3968
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type
'Oxford Diffraction Gemini A Ultra diffractometer'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube with Enhance optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0525
_diffrn_reflns_av_sigmaI/netI    0.0744
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            51986
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.88
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.483
_exptl_absorpt_correction_T_max  0.468
_exptl_absorpt_correction_T_min  0.347
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   CrysAlisPro
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.663
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3392
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.938
_refine_diff_density_min         -2.070
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.850
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     831
_refine_ls_number_reflns         11965
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.850
_refine_ls_R_factor_all          0.0561
_refine_ls_R_factor_gt           0.0295
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0257P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0531
_refine_ls_wR_factor_ref         0.0557
_reflns_number_gt                7999
_reflns_number_total             11965
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om1006769_si_002.cif
_cod_data_source_block           sd296_compound_5
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4066844