Catalyst- and solvent-free conditions as an environmentally benign approach to 4-aryl-3-cyano-hexahydro-4H-1,2-benzoxazine-2-oxides
Bellachioma, Gianfranco; Castrica, Luca; Fringuelli, Francesco; Pizzo, Ferdinando; Vaccaro, Luigi; Green Chemistry 10 (2008) 327–; doi:10.1039/b712858d

data_7215777
_publ_section_title
;
 Catalyst- and solvent-free conditions as an environmentally benign
 approach to 4-aryl-3-cyano-hexahydro-4H-1,2-benzoxazine-2-oxides
;
_journal_issue                   3
_journal_name_full               'Green Chemistry'
_journal_page_first              327
_journal_paper_doi               10.1039/b712858d
_journal_volume                  10
_journal_year                    2008
_chemical_formula_moiety         'C18 H24 N2 O3 Si'
_chemical_formula_sum            'C18 H24 N2 O3 Si'
_chemical_formula_weight         344.48
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_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                102.062(17)
_cell_angle_beta                 105.681(17)
_cell_angle_gamma                103.638(17)
_cell_formula_units_Z            2
_cell_length_a                   9.893(2)
_cell_length_b                   10.366(2)
_cell_length_c                   10.379(2)
_cell_measurement_temperature    295(2)
_cell_volume                     952.6(4)
_computing_cell_refinement       'CRYSALIS (CCD 171) software'
_computing_data_collection       'XCALIBUR (Kuma4CCD) diffractometer'
_computing_data_reduction        'CRYSALIS (CCD 171) software'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_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  0.0960
_diffrn_reflns_av_sigmaI/netI    0.2823
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            14614
_diffrn_reflns_theta_full        29.47
_diffrn_reflns_theta_max         29.47
_diffrn_reflns_theta_min         4.10
_exptl_absorpt_coefficient_mu    0.140
_exptl_absorpt_correction_T_max  0.9765
_exptl_absorpt_correction_T_min  0.9644
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   r.h.blessing,actacryst.(1995),a5
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.201
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             368
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.151
_refine_diff_density_min         -0.118
_refine_diff_density_rms         0.029
_refine_ls_extinction_coef       0.0067(14)
_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   0.876
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     174
_refine_ls_number_reflns         5292
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.876
_refine_ls_R_factor_all          0.2485
_refine_ls_R_factor_gt           0.0409
_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^)+(0.0207P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0550
_refine_ls_wR_factor_ref         0.0772
_reflns_number_gt                3156
_reflns_number_total             5292
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b712858d.txt
_cod_data_source_block           11a
_cod_database_code               7215777