Cobalt-Catalyzed Intermolecular [2 + 2 + 2] Cycloaddition for the Synthesis of 1,3-Cyclohexadienes
Gerhard Hilt; Anna Paul; Klaus Harms; Journal of Organic Chemistry 73 (2008) 5187–5190; doi:10.1021/jo800735x

data_4023519
_publ_section_title
;
 Cobalt-Catalyzed Intermolecular [2 + 2 + 2] Cycloaddition
 for the Synthesis of 1,3-Cyclohexadienes
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              5187
_journal_page_last               5190
_journal_paper_doi               10.1021/jo800735x
_journal_volume                  73
_journal_year                    2008
_chemical_formula_moiety         'C26 H28 O5'
_chemical_formula_sum            'C26 H28 O5'
_chemical_formula_weight         420.48
_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, O-H difmap'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                68.579(12)
_cell_angle_beta                 70.743(12)
_cell_angle_gamma                78.726(13)
_cell_formula_units_Z            2
_cell_length_a                   9.5186(11)
_cell_length_b                   10.0427(11)
_cell_length_c                   13.5127(15)
_cell_measurement_reflns_used    7872
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      2.2
_cell_volume                     1131.1(2)
_computing_cell_refinement       'STOE CELL'
_computing_data_collection       'STOE EXPOSE'
_computing_data_reduction        'STOE INTEGRATE'
_computing_molecular_graphics    'DIAMOND 3.1'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1993)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.936
_diffrn_measured_fraction_theta_max 0.936
_diffrn_measurement_device_type  'STOE IPDS'
_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  0.0280
_diffrn_reflns_av_sigmaI/netI    0.0314
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            10208
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.29
_exptl_absorpt_coefficient_mu    0.085
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.235
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             448
_exptl_crystal_size_max          0.51
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.261
_refine_diff_density_min         -0.332
_refine_diff_density_rms         0.036
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    'constr., O-H ref'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     313
_refine_ls_number_reflns         3720
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0703
_refine_ls_R_factor_gt           0.0524
_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^)+(0.0835P)^2^+0.1838P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1418
_refine_ls_wR_factor_ref         0.1504
_reflns_number_gt                2668
_reflns_number_total             3720
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo800735x-File001_1.cif
_cod_data_source_block           4h
_cod_database_code               4023519