4-Methoxy-11-oxo-5-azabenzo[<i>b</i>]fluorene <i>N</i>-Oxide and its Free Base
Kubicki, M.; Borowiak, T.; Antkowiak, W. Z.; Acta Crystallographica Section C 51 (1995) 462–465; doi:10.1107/S0108270194010528

data_2003227
_publ_section_title
;
 4-Methoxy-11-oxo-5-azabenzo[<i>b</i>]fluorene <i>N</i>-Oxide and its
 Free Base
;
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              462
_journal_page_last               465
_journal_paper_doi               10.1107/S0108270194010528
_journal_volume                  51
_journal_year                    1995
_chemical_formula_moiety         'C17 H11 N O3'
_chemical_formula_sum            'C17 H11 N O3'
_chemical_formula_weight         277.27
_chemical_name_systematic
;
1-methoxy-5-oxo-11-azabenzo[b]fluorene-11-oxide
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   21.023(1)
_cell_length_b                   14.907(1)
_cell_length_c                   8.2059(7)
_cell_measurement_reflns_used    15
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      47.15
_cell_measurement_theta_min      18.06
_cell_volume                     2571.6(3)
_computing_cell_refinement       'P2~1~ Standard'
_computing_data_collection       'P2~1~ Standard'
_computing_data_reduction        'PRADIR (Jask\'olski, 1990)'
_computing_molecular_graphics    'Stereochemical Workstation (1989)'
_computing_publication_material  'SHELXL-93 (Sheldrick, 1994)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1994)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Syntex P2~1~'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  'not determined'
_diffrn_reflns_av_sigmaI/netI    0.0173
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            1204
_diffrn_reflns_theta_max         57.28
_diffrn_reflns_theta_min         4.21
_diffrn_standards_decay_%        2.4
_diffrn_standards_interval_count 100
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.815
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.432
_exptl_crystal_description       prism
_exptl_crystal_F_000             1152
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.153
_refine_diff_density_min         -0.109
_refine_ls_extinction_coef       0.0022(3)
_refine_ls_extinction_method
'F~c~^*^ = kF~c~[1+0.001xF~c~^2^\l^3^/sin(2\q)]'
_refine_ls_goodness_of_fit_all   1.087
_refine_ls_goodness_of_fit_obs   1.087
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     191
_refine_ls_number_reflns         1200
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.130
_refine_ls_restrained_S_obs      1.087
_refine_ls_R_factor_all          0.0387
_refine_ls_R_factor_obs          0.0380
_refine_ls_shift/esd_max         <0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
;calc w = 1/[\s^2^(F~o~^2^)+(0.0276P)^2^+1.5593P] where P =
(F~o~^2^+2F~c~^2^)/3
;
_refine_ls_wR_factor_all         0.0859
_refine_ls_wR_factor_obs         0.0825
_reflns_number_observed          1199
_reflns_number_total             1204
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ab1206.cif
_cod_data_source_block           1
_cod_database_code               2003227