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_4119950
_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_sum            'C31 H45 Co O6 S Si'
_chemical_formula_weight         632.75
_chemical_name_systematic
; 
 ? 
;
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_atom_sites_solution_secondary   difmap
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_cell_formula_units_Z            16
_cell_length_a                   12.3188(8)
_cell_length_b                   26.3035(16)
_cell_length_c                   39.777(3)
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_cell_measurement_temperature    100(2)
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_cell_measurement_theta_min      3.40
_cell_volume                     12582.6(15)
_computing_cell_refinement       'Bruker SAINT'
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_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 0.972
_diffrn_measured_fraction_theta_max 0.883
_diffrn_measurement_device_type  'Bruker APEX-II 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     1.54184
_diffrn_reflns_av_R_equivalents  0.1217
_diffrn_reflns_av_sigmaI/netI    0.1671
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -31
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_diffrn_reflns_limit_l_min       -42
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_diffrn_reflns_theta_min         1.14
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_exptl_absorpt_correction_T_max  0.8502
_exptl_absorpt_correction_T_min  0.3136
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.336
_exptl_crystal_description       Plate
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_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
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_refine_ls_number_reflns         41449
_refine_ls_number_restraints     1200
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_refine_ls_R_factor_all          0.2403
_refine_ls_R_factor_gt           0.1594
_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^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3616
_refine_ls_wR_factor_ref         0.4205
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_reflns_threshold_expression     >2sigma(I)
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_cod_database_code               4119950