Chemistry at the Alkyne-Carbene Intersection: A Metallacyclobutene-η3-Vinylcarbene Equilibration
Joseph M. O'Connor; Kim K. Baldridge; Carmen L. Vélez; Arnold L. Rheingold; Curtis E. Moore; Journal of the American Chemical Society 135 (2013) 8826–8829; doi:10.1021/ja4039483

data_4119948
_publ_section_title
;
 Chemistry at the Alkyne-Carbene Intersection: A
 Metallacyclobutene-\h3-Vinylcarbene Equilibration
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8826
_journal_page_last               8829
_journal_paper_doi               10.1021/ja4039483
_journal_volume                  135
_journal_year                    2013
_chemical_formula_moiety         'C38 H40 Co O4 P S Si'
_chemical_formula_sum            'C38 H40 Co O4 P S Si'
_chemical_formula_weight         710.75
_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                 100.763(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.847(3)
_cell_length_b                   18.614(5)
_cell_length_c                   18.744(5)
_cell_measurement_reflns_used    7806
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.3
_cell_measurement_theta_min      1.6
_cell_volume                     3375.2(16)
_computing_cell_refinement       'Bruker SHELL'
_computing_data_collection       'Bruker SHELL'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    ORTEP-32
_computing_publication_material  WINGX
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.932
_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  0.0671
_diffrn_reflns_av_sigmaI/netI    0.0732
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            28605
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         1.56
_exptl_absorpt_coefficient_mu    0.694
_exptl_absorpt_correction_T_max  0.9863
_exptl_absorpt_correction_T_min  0.8971
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.399
_exptl_crystal_description       plate
_exptl_crystal_F_000             1488
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.654
_refine_diff_density_min         -0.338
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     419
_refine_ls_number_reflns         7806
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.0760
_refine_ls_R_factor_gt           0.0459
_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^)+(0.0535P)^2^+0.0478P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1017
_refine_ls_wR_factor_ref         0.1139
_reflns_number_gt                5549
_reflns_number_total             7806
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja4039483_si_002_2.cif
_cod_data_source_block           rlh2045
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4119948