Basic alumina-supported highly effective Suzuki–Miyaura cross-coupling reaction under microwave irradiation: application to fused tricyclic oxa-aza-quinolones
Saha, Pritam; Naskar, Subhendu; Paira, Priyankar; Hazra, Abhijit; Sahu, Krishnendu B.; Paira, Rupankar; Banerjee, Sukdeb; Mondal, Nirup B.; Green Chemistry 11 (2009) 931–; doi:10.1039/b902916h

data_7201002
_publ_section_title
;
 Basic alumina-supported highly effective Suzuki--Miyaura
 cross-coupling reaction under microwave irradiation: application to
 fused tricyclic oxa-aza-quinolones
;
_journal_issue                   7
_journal_name_full               'Green Chemistry'
_journal_page_first              931
_journal_paper_doi               10.1039/b902916h
_journal_volume                  11
_journal_year                    2009
_chemical_formula_sum            'C19 H13 N O2 S2'
_chemical_formula_weight         351.42
_chemical_name_common            oxazinoquinoline
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                83.143(5)
_cell_angle_beta                 72.938(4)
_cell_angle_gamma                64.907(4)
_cell_formula_units_Z            2
_cell_length_a                   8.655(2)
_cell_length_b                   9.619(3)
_cell_length_c                   10.727(3)
_cell_measurement_reflns_used    7752
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.46
_cell_measurement_theta_min      1.99
_cell_volume                     773.2(4)
_computing_cell_refinement       'Kappa Apex 2'
_computing_data_collection       'Kappa Apex 2'
_computing_data_reduction        'Kappa Apex 2'
_computing_molecular_graphics    PLATON(Spek,2004)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.883
_diffrn_measured_fraction_theta_max 0.883
_diffrn_measurement_device       'Kappa Apex 2 CCD system'
_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  0.0234
_diffrn_reflns_av_sigmaI/netI    0.0309
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            7752
_diffrn_reflns_theta_full        28.46
_diffrn_reflns_theta_max         28.46
_diffrn_reflns_theta_min         1.99
_diffrn_standards_decay_%        n/a
_diffrn_standards_interval_count n/a
_diffrn_standards_interval_time  n/a
_diffrn_standards_number         n/a
_exptl_absorpt_coefficient_mu    0.356
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Yellowish
_exptl_crystal_density_diffrn    1.509
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Rectangular
_exptl_crystal_F_000             364
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.389
_refine_diff_density_min         -0.309
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     214
_refine_ls_number_reflns         3454
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.114
_refine_ls_R_factor_all          0.0676
_refine_ls_R_factor_gt           0.0481
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
_refine_ls_weighting_details
w=1/[\s^2^(Fo^2^)+(0.0662P)^2^+0.1787P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1288
_refine_ls_wR_factor_ref         0.1416
_reflns_number_gt                2479
_reflns_number_total             3454
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b902916h.txt
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7201002