UV Promoted Phenanthridine Syntheses from Oxime Carbonate Derived Iminyl Radicals
Roy T. McBurney; Alexandra M. Z. Slawin; Laura A. Smart; Yanping Yu; John C. Walton; Chem. Commun. 47 (2011) 7974–; doi:10.1039/c1cc12720a

data_7106653
_publ_section_title
;
 UV Promoted Phenanthridine Syntheses from Oxime Carbonate Derived Iminyl
 Radicals
;
_journal_name_full               'Chem. Commun.'
_journal_page_first              7974
_journal_paper_doi               10.1039/c1cc12720a
_journal_volume                  47
_journal_year                    2011
_chemical_formula_moiety         'C14 H10 N2 O2'
_chemical_formula_sum            'C14 H10 N2 O2'
_chemical_formula_weight         238.24
_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                 96.36(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   4.469(3)
_cell_length_b                   13.268(10)
_cell_length_c                   18.459(16)
_cell_measurement_reflns_used    1066
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      68.5
_cell_measurement_theta_min      21.6
_cell_volume                     1087.8(14)
_computing_cell_refinement       'CrystalClear (Rigaku Corp., 2004)'
_computing_data_collection       'CrystalClear (Rigaku Corp., 2004)'
_computing_data_reduction        'CrystalClear (Rigaku Corp., 2004)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  CCD
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  confocal
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1630
_diffrn_reflns_av_sigmaI/netI    0.0708
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            13762
_diffrn_reflns_theta_full        67.00
_diffrn_reflns_theta_max         68.25
_diffrn_reflns_theta_min         4.11
_exptl_absorpt_coefficient_mu    0.816
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.516
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.455
_exptl_crystal_description       Prism
_exptl_crystal_F_000             496
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.382
_refine_diff_density_min         -0.384
_refine_diff_density_rms         0.085
_refine_ls_extinction_coef       0.028(9)
_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   1.244
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     165
_refine_ls_number_reflns         1978
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.244
_refine_ls_R_factor_all          0.1570
_refine_ls_R_factor_gt           0.1223
_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^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3345
_refine_ls_wR_factor_ref         0.3712
_reflns_number_gt                1317
_reflns_number_total             1978
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1cc12720a.txt
_cod_data_source_block           5d
_cod_original_cell_volume        1087.8(15)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7106653