Dibenzoxazepinium ylides: facile access and 1,3-dipolar cycloaddition reactions.
Khlebnikov, Alexander F.; Novikov, Mikhail S.; Petrovskii, Petr P.; Magull, Joerg; Ringe, Arne; Organic letters 11 (2009) 979–982; doi:10.1021/ol802813a

data_1503779
_publ_section_title
;
 Dibenzoxazepinium ylides: facile access and 1,3-dipolar cycloaddition
 reactions.
;
_journal_issue                   4
_journal_name_full               'Organic letters'
_journal_page_first              979
_journal_page_last               982
_journal_paper_doi               10.1021/ol802813a
_journal_volume                  11
_journal_year                    2009
_chemical_formula_sum            'C20 H15 N O'
_chemical_formula_weight         285.33
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 118.75(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   20.217(4)
_cell_length_b                   8.3327(17)
_cell_length_c                   20.468(4)
_cell_measurement_temperature    133(2)
_cell_volume                     3023.0(14)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0898
_diffrn_reflns_av_sigmaI/netI    0.0426
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            69859
_diffrn_reflns_theta_full        25.85
_diffrn_reflns_theta_max         25.85
_diffrn_reflns_theta_min         1.97
_exptl_absorpt_coefficient_mu    0.077
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.254
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1200
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.233
_refine_diff_density_min         -0.195
_refine_diff_density_rms         0.036
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.990
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     397
_refine_ls_number_reflns         5827
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.990
_refine_ls_R_factor_all          0.0822
_refine_ls_R_factor_gt           0.0543
_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^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1393
_refine_ls_wR_factor_ref         0.1537
_reflns_number_gt                4412
_reflns_number_total             5827
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol802813a_si_001.cif
_cod_data_source_block           p1
_cod_original_cell_volume        3023.0(11)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               1503779