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_7106652
_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_absolute_configuration ad
_chemical_formula_moiety         'C17 H16 Cl N O3'
_chemical_formula_sum            'C17 H16 Cl N O3'
_chemical_formula_weight         317.76
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 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                 95.759(14)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   24.039(14)
_cell_length_b                   7.017(5)
_cell_length_c                   19.280(12)
_cell_measurement_reflns_used    1443
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      68.6
_cell_measurement_theta_min      21.3
_cell_volume                     3236(4)
_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 0.996
_diffrn_measured_fraction_theta_max 0.989
_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  0.2075
_diffrn_reflns_av_sigmaI/netI    0.1329
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            20550
_diffrn_reflns_theta_full        67.00
_diffrn_reflns_theta_max         68.08
_diffrn_reflns_theta_min         2.30
_exptl_absorpt_coefficient_mu    2.191
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.756
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.305
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1328
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.723
_refine_diff_density_min         -0.600
_refine_diff_density_rms         0.105
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.09(5)
_refine_ls_extinction_coef       0.0053(8)
_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   1.203
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     400
_refine_ls_number_reflns         5616
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.203
_refine_ls_R_factor_all          0.1656
_refine_ls_R_factor_gt           0.1423
_refine_ls_shift/su_max          0.075
_refine_ls_shift/su_mean         0.020
_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          0.3619
_refine_ls_wR_factor_ref         0.3976
_reflns_number_gt                3630
_reflns_number_total             5616
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1cc12720a.txt
_cod_data_source_block           4f
_cod_original_sg_symbol_H-M      C2
_cod_database_code               7106652