Addition of Dissimilar Carbenes across an Unsymmetrically Substituted Alkyne: Regio- and Stereoselective Synthesis of Trisubstituted 1,3-Dienes
O’Connor, Joseph M.; Chen, Ming-Chou; Holland, Ryan L.; Rheingold, Arnold L.; Organometallics 30 (2011) 369–; doi:10.1021/om1007314

data_4063646
_publ_section_title
;
 Addition of Dissimilar Carbenes across an Unsymmetrically Substituted
 Alkyne: Regio- and Stereoselective Synthesis of Trisubstituted 1,3-Dienes
;
_journal_issue                   3
_journal_name_full               Organometallics
_journal_page_first              369
_journal_paper_doi               10.1021/om1007314
_journal_volume                  30
_journal_year                    2011
_chemical_formula_moiety         'C20 H21 Co O5 S'
_chemical_formula_sum            'C20 H21 Co O5 S'
_chemical_formula_weight         432.36
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                94.7630(11)
_cell_angle_beta                 108.9571(7)
_cell_angle_gamma                92.8772(2)
_cell_formula_units_Z            2
_cell_length_a                   8.7427(2)
_cell_length_b                   10.9158(2)
_cell_length_c                   10.9738(2)
_cell_measurement_reflns_used    4208
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      28.3
_cell_measurement_theta_min      1.9
_cell_volume                     983.73(3)
_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-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.860
_diffrn_measurement_device_type  'Bruker APEX CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0279
_diffrn_reflns_av_sigmaI/netI    0.0517
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            6498
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.27
_diffrn_reflns_theta_min         1.88
_exptl_absorpt_coefficient_mu    1.006
_exptl_absorpt_correction_T_max  0.8242
_exptl_absorpt_correction_T_min  0.6891
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.460
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             448
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.508
_refine_diff_density_min         -0.406
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     246
_refine_ls_number_reflns         4208
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0435
_refine_ls_R_factor_gt           0.0395
_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^)+(0.0933P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1296
_refine_ls_wR_factor_ref         0.1324
_reflns_number_gt                3740
_reflns_number_total             4208
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om1007314_si_002.cif
_cod_data_source_block           jmo35
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4063646