Contrasting Responses of Pyrido[2,1-a]isoindol-6-ones and Their Sultam Counterparts to Photochemical Activation
Leo A. Paquette; Robert D. Dura; Isabelle Modolo; Journal of Organic Chemistry 74 (2009) 1982–1987; doi:10.1021/jo802476c

data_4024363
_publ_contact_author_address
;
Department of Chemistry
Ohio State University
Columbus, OH 43210
;
_publ_contact_author_name        'Paquette, Leo'
_publ_section_title
;
Contrasting Responses of Pyrido[2,1-a]isoindol-6-ones and Their Sultam
Counterparts to Photochemical Activation
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              1982
_journal_page_last               1987
_journal_paper_doi               10.1021/jo802476c
_journal_volume                  74
_journal_year                    2009
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C26 H22 N2 O4'
_chemical_formula_sum            'C26 H22 N2 O4'
_chemical_formula_weight         426.46
_chemical_name_common            'Paquette 1598'
_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
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_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                101.625(3)
_cell_angle_beta                 95.611(3)
_cell_angle_gamma                98.740(3)
_cell_formula_units_Z            4
_cell_length_a                   8.6296(1)
_cell_length_b                   13.9375(1)
_cell_length_c                   18.6870(2)
_cell_measurement_reflns_used    7599
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.028
_cell_measurement_theta_min      2.037
_cell_measurement_wavelength     0.71073
_cell_volume                     2156.68(4)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_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      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      0.109142E-1
_diffrn_orient_matrix_UB_12      -0.145302E-1
_diffrn_orient_matrix_UB_13      0.503385E-1
_diffrn_orient_matrix_UB_21      0.67048E-1
_diffrn_orient_matrix_UB_22      0.670638E-1
_diffrn_orient_matrix_UB_23      0.198558E-1
_diffrn_orient_matrix_UB_31      -0.968358E-1
_diffrn_orient_matrix_UB_32      0.287893E-1
_diffrn_orient_matrix_UB_33      0.10492E-1
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.028
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            51609
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.61
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    0.089
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.313
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'trapezoid-shaped chunk'
_exptl_crystal_F_000             896
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.235
_refine_diff_density_min         -0.173
_refine_diff_density_rms         0.032
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     597
_refine_ls_number_reflns         7626
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.06
_refine_ls_R_factor_gt           0.0406
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0609P)^2^+0.2995P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1071
_refine_ls_wR_factor_ref         0.1169
_reflns_number_gt                5655
_reflns_number_total             7626
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo802476c_si_002.cif
_cod_data_source_block           Paquette1598
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4024363