Preparation of Seven- and Eight-Membered Boron Heterocycles from Different Salen Ligands and Arylboronic Acids
Mario Sánchez; Herbert Höpfl; Maria-Eugenia Ochoa; Norberto Farfán; Rosa Santillan; Susana Rojas-Lima; Inorganic Chemistry 40 (2001) 6405–6412; doi:10.1021/ic010580g

data_4320656
_publ_contact_author_address
;
Centro de Investigaciones Qu\'imicas
Universidad Aut\'onoma del Estado de Morelos
Av. Universidad 1001
C.P. 62210 Cuernavaca
Mexico 
;
_publ_contact_author_email       ' hhopfl@buzon.uaem.mx '
_publ_contact_author_fax         ' +52 73 29 79 98 '
_publ_contact_author_name        'Herbert H\"opfl'
_publ_contact_author_phone       ' +52 73 29 79 97 '
_publ_section_title
;
 Preparation of Seven- and Eight-Membered Boron Heterocycles from
 Different Salen Ligands and Arylboronic Acids
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6405
_journal_page_last               6412
_journal_paper_doi               10.1021/ic010580g
_journal_volume                  40
_journal_year                    2001
_chemical_formula_moiety         'C35 H40 B2 N2 O4'
_chemical_formula_sum            'C35 H40 B2 N2 O4'
_chemical_formula_weight         574.31
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_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            4
_cell_length_a                   17.784(4)
_cell_length_b                   7.9650(15)
_cell_length_c                   23.028(5)
_cell_measurement_temperature    293(2)
_cell_volume                     3261.9(12)
_computing_cell_refinement       'SAINT, version 6.01, 1999'
_computing_data_collection       'Smart, version 5.057c, 1997-1998'
_computing_data_reduction        'SAINT, version 6.01, 1999'
_computing_molecular_graphics    'SHELXTL-NT, version 5.10, 1999'
_computing_publication_material  'SHELXTL-NT, version 5.10, 1999'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker Smart 6000'
_diffrn_measurement_method       CCD
_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  0.0913
_diffrn_reflns_av_sigmaI/netI    0.1126
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            19159
_diffrn_reflns_theta_full        25.10
_diffrn_reflns_theta_max         25.10
_diffrn_reflns_theta_min         1.77
_exptl_absorpt_coefficient_mu    0.075
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.170
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cube
_exptl_crystal_F_000             1224
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.106
_refine_diff_density_min         -0.099
_refine_diff_density_rms         0.025
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   1.3(19)
_refine_ls_extinction_coef       0.0032(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.748
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     369
_refine_ls_number_reflns         5398
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.748
_refine_ls_R_factor_all          0.1660
_refine_ls_R_factor_gt           0.0457
_refine_ls_shift/su_max          0.022
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0358P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0810
_refine_ls_wR_factor_ref         0.1063
_reflns_number_gt                1820
_reflns_number_total             5398
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010580g_3.cif
_cod_data_source_block           srl11
_cod_original_cell_volume        3261.8(11)
_cod_database_code               4320656