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_4119947
_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         'C45 H54 Co O4 P S Si'
_chemical_formula_sum            'C45 H54 Co O4 P S Si'
_chemical_formula_weight         808.93
_chemical_name_common            CLV30_4
_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                62.211(10)
_cell_angle_beta                 83.252(11)
_cell_angle_gamma                85.344(10)
_cell_formula_units_Z            2
_cell_length_a                   11.880(9)
_cell_length_b                   14.995(12)
_cell_length_c                   15.155(12)
_cell_measurement_reflns_used    9913
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.8
_cell_measurement_theta_min      1.5
_cell_volume                     2371(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      373(2)
_diffrn_measured_fraction_theta_full 0.915
_diffrn_measured_fraction_theta_max 0.803
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0518
_diffrn_reflns_av_sigmaI/netI    0.0572
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            27842
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.79
_diffrn_reflns_theta_min         1.53
_exptl_absorpt_coefficient_mu    0.501
_exptl_absorpt_correction_T_max  0.9020
_exptl_absorpt_correction_T_min  0.8323
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.133
_exptl_crystal_description       block
_exptl_crystal_F_000             856
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.21
_refine_diff_density_max         1.364
_refine_diff_density_min         -0.361
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.961
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     486
_refine_ls_number_reflns         9913
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.961
_refine_ls_R_factor_all          0.0660
_refine_ls_R_factor_gt           0.0487
_refine_ls_shift/su_max          0.027
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0731P)^2^+0.7106P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1328
_refine_ls_wR_factor_ref         0.1425
_reflns_number_gt                7159
_reflns_number_total             9913
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja4039483_si_002_1.cif
_cod_data_source_block           clv30_4
_cod_database_code               4119947