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_4119949
_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         'C32 H44 Co2 O4 S Si'
_chemical_formula_sum            'C32 H44 Co2 O4 S Si'
_chemical_formula_weight         670.68
_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                 98.015(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.2488(8)
_cell_length_b                   17.4041(13)
_cell_length_c                   14.7075(11)
_cell_measurement_reflns_used    9854
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      67.01
_cell_measurement_theta_min      3.64
_cell_volume                     3104.7(4)
_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      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'Bruker APEX CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'Double Bounce Multilayer Mirror'
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0490
_diffrn_reflns_av_sigmaI/netI    0.0294
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            34277
_diffrn_reflns_theta_full        60.00
_diffrn_reflns_theta_max         67.52
_diffrn_reflns_theta_min         3.64
_exptl_absorpt_coefficient_mu    9.645
_exptl_absorpt_correction_T_max  0.7607
_exptl_absorpt_correction_T_min  0.1804
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'Dark Red'
_exptl_crystal_density_diffrn    1.435
_exptl_crystal_description       Needle
_exptl_crystal_F_000             1408
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.528
_refine_diff_density_min         -0.289
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     369
_refine_ls_number_reflns         5457
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0403
_refine_ls_R_factor_gt           0.0332
_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^)+(0.0458P)^2^+2.0964P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0802
_refine_ls_wR_factor_ref         0.0848
_reflns_number_gt                4864
_reflns_number_total             5457
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja4039483_si_002_3.cif
_cod_data_source_block           clv67_7
_cod_database_code               4119949