BF3•Et2O-Mediated Intramolecular Cyclization of Unsaturated Amides: Convenient Synthesis of Dihydroquinolin-2-one-BF2 Complexes
Liu, Xu; Zhang, Qian; Xin, Xiaoqing; Zhang, Rui; Zhang, Ning; Liang, Yongjiu; Dong, Dewen; RSC Advances 4 (2014) 36234–36240; doi:10.1039/C4RA06151A

data_7217638
_publ_section_title
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 BF3&#x2022;Et2O-Mediated Intramolecular Cyclization of Unsaturated
 Amides: Convenient Synthesis of Dihydroquinolin-2-one-BF2 Complexes
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_journal_issue                   68
_journal_name_full               'RSC Advances'
_journal_page_first              36234
_journal_page_last               36240
_journal_paper_doi               10.1039/C4RA06151A
_journal_volume                  4
_journal_year                    2014
_chemical_formula_sum            'C45 H38 B2 Cl2 F4 N2 O6'
_chemical_formula_weight         871.29
_chemical_melting_point          153(2)
_chemical_name_common
8-(2-Chlorophenyl)-2,2-difluoro-7-(4-methoxyphenyl)-4-methyl-7,8-dihydro-2H-[1,3,2]dioxaborinino[4,5-b]pyridin-1-ium-2-uide
_chemical_name_systematic        ?
_space_group_IT_number           2
_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                101.954(5)
_cell_angle_beta                 104.028(5)
_cell_angle_gamma                98.284(5)
_cell_formula_units_Z            1
_cell_length_a                   7.643(5)
_cell_length_b                   12.269(5)
_cell_length_c                   12.840(5)
_cell_measurement_temperature    293(2)
_cell_volume                     1118.6(10)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.975
_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  0.0123
_diffrn_reflns_av_sigmaI/netI    0.0244
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            6123
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.07
_diffrn_reflns_theta_min         1.73
_exptl_absorpt_coefficient_mu    0.210
_exptl_crystal_density_diffrn    1.293
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             450
_refine_diff_density_max         0.651
_refine_diff_density_min         -0.331
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         4318
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.1055
_refine_ls_R_factor_gt           0.0884
_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^)+(0.1848P)^2^+0.6504P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2757
_refine_ls_wR_factor_ref         0.2992
_reflns_number_gt                3256
_reflns_number_total             4318
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c4ra06151a2.cif
_cod_data_source_block           p
_cod_depositor_comments
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The following automatic conversions were performed:

'_chemical_melting_point' value '151-155' was changed to '153(2)' -
the average value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_sg_symbol_H-M      p-1
_cod_database_code               7217638