An Opened Route to 1,3-Dimethylenecyclobutanes via Sequential Ruthenium-Catalyzed [2 + 2] Cycloaddition of Allenyl Boronate and Palladium Suzuki Coupling
Emilio Bustelo; Carine Guérot; Alain Hercouet; Bertrand Carboni; Loïc Toupet; Pierre H. Dixneuf; Journal of the American Chemical Society 127 (2005) 11582–11583; doi:10.1021/ja051930r

data_4111866
_publ_section_title
;
 An Opened Route to 1,3-Dimethylenecyclobutanes via Sequential
 Ruthenium-Catalyzed [2 + 2] Cycloaddition of Allenyl Boronate and
 Palladium Suzuki Coupling
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11582
_journal_page_last               11583
_journal_paper_doi               10.1021/ja051930r
_journal_volume                  127
_journal_year                    2005
_chemical_formula_sum            'C9 H8'
_chemical_formula_weight         116.15
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   7.6184(6)
_cell_length_b                   9.5951(7)
_cell_length_c                   17.0181(9)
_cell_measurement_temperature    293(2)
_cell_volume                     1244.01(15)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Nonius (1999)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'PLATON_(Spek, 1998)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-97_(Altomare & al., 1998)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 19.24
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.949
_diffrn_measurement_device_type  Nonius_KappaCCD
_diffrn_measurement_method       'Area detector scans (see text)'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0558
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            1526
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.68
_diffrn_reflns_theta_min         2.39
_exptl_absorpt_coefficient_mu    0.070
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourles
_exptl_crystal_density_diffrn    1.240
_exptl_crystal_description       block
_exptl_crystal_F_000             496
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.278
_refine_diff_density_min         -0.270
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     82
_refine_ls_number_reflns         1526
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.1106
_refine_ls_R_factor_gt           0.0671
_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^)+(0.0973P)^2^+0.5668P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1599
_refine_ls_wR_factor_ref         0.1953
_reflns_number_gt                992
_reflns_number_total             1526
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja051930rsi20050710_105350.cif
_cod_data_source_block           eb20
_cod_database_code               4111866