Pd-catalyzed borylative cyclisation of 1,7-enynes
Diego Cardenas; Elena Bunuel; Virtudes Pardo-Rodriguez; Daniel Collado-Sanz; Chem.Commun. 48 (2012) 10517–; doi:10.1039/c2cc34468h

data_7108479
_publ_section_title
;
 Pd-catalyzed borylative cyclisation of 1,7-enynes
;
_journal_name_full               Chem.Commun.
_journal_page_first              10517
_journal_paper_doi               10.1039/c2cc34468h
_journal_volume                  48
_journal_year                    2012
_chemical_formula_sum            'C27 H35 B O6 S2'
_chemical_formula_weight         530.48
_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                 96.757(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.4977(5)
_cell_length_b                   20.3568(8)
_cell_length_c                   10.5584(5)
_cell_measurement_reflns_used    7002
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.54
_cell_measurement_theta_min      2.59
_cell_volume                     2667.5(2)
_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 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w 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  0.0385
_diffrn_reflns_av_sigmaI/netI    0.0394
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            26845
_diffrn_reflns_theta_full        26.78
_diffrn_reflns_theta_max         26.78
_diffrn_reflns_theta_min         1.64
_exptl_absorpt_coefficient_mu    0.240
_exptl_absorpt_correction_T_max  0.9718
_exptl_absorpt_correction_T_min  0.8957
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.321
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1128
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.266
_refine_diff_density_min         -0.784
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     330
_refine_ls_number_reflns         5640
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.1278
_refine_ls_R_factor_gt           0.0952
_refine_ls_shift/su_max          3.409
_refine_ls_shift/su_mean         0.278
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1523P)^2^+8.1432P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2551
_refine_ls_wR_factor_ref         0.2907
_reflns_number_gt                4114
_reflns_number_total             5640
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc34468h.txt
_cod_data_source_block           datos
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7108479