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_4063645
_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         'C34 H40 Co O6 S'
_chemical_formula_sum            'C34 H40 Co O6 S'
_chemical_formula_weight         635.65
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 97.172(13)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.305(2)
_cell_length_b                   14.764(3)
_cell_length_c                   22.592(3)
_cell_measurement_reflns_used    4861
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      22.5
_cell_measurement_theta_min      2.1
_cell_volume                     3741.3(11)
_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      298(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0550
_diffrn_reflns_av_sigmaI/netI    0.1305
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            6257
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         2.13
_exptl_absorpt_coefficient_mu    0.551
_exptl_absorpt_correction_T_max  0.8521
_exptl_absorpt_correction_T_min  0.8097
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.129
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1340
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.545
_refine_diff_density_min         -0.406
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     387
_refine_ls_number_reflns         4861
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.1571
_refine_ls_R_factor_gt           0.0760
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1014P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1731
_refine_ls_wR_factor_ref         0.2134
_reflns_number_gt                2603
_reflns_number_total             4861
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om1007314_si_002.cif
_cod_data_source_block           jmo25
_cod_original_cell_volume        3741.1(12)
_cod_original_sg_symbol_Hall     -P2yn
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               4063645