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_4066842
_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         'C35 H27 Au Cl O P,C H2 Cl2'
_chemical_formula_sum            'C36 H29 Au Cl3 O P'
_chemical_formula_weight         811.88
_chemical_name_systematic
;
 ?
;
_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                 112.921(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.5161(3)
_cell_length_b                   17.2666(4)
_cell_length_c                   15.3084(4)
_cell_measurement_reflns_used    11101
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.56
_cell_measurement_theta_min      2.87
_cell_volume                     3290.54(15)
_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 0.984
_diffrn_measured_fraction_theta_max 0.847
_diffrn_measurement_device_type
'Oxford Diffraction Gemini A Ultra diffractometer'
_diffrn_measurement_method       'thick-slice \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  0.0347
_diffrn_reflns_av_sigmaI/netI    0.0551
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            22102
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.62
_diffrn_reflns_theta_min         2.87
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.791
_exptl_absorpt_correction_T_max  0.534
_exptl_absorpt_correction_T_min  0.358
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   CrysAlisPro
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.639
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1592
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.823
_refine_diff_density_min         -1.363
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.920
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     353
_refine_ls_number_reflns         7151
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.920
_refine_ls_R_factor_all          0.0450
_refine_ls_R_factor_gt           0.0304
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0382P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0670
_refine_ls_wR_factor_ref         0.0690
_reflns_number_gt                5260
_reflns_number_total             7151
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om1006769_si_002.cif
_cod_data_source_block           sd295_compound_4b
_cod_original_cell_volume        3290.54(14)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4066842