Ethyl 7-oxo-7<i>H</i>-benzo[<i>de</i>]imidazo[5,1-<i>a</i>]isoquinoline-11-carboxylate–trifluoroacetic acid (1/1)
Stibrany, Robert T.; Potenza, Joseph A.; Acta Crystallographica Section E 69 (2013) o977–o978; doi:10.1107/S1600536813013834

data_2237839
_publ_section_title
;
 Ethyl
 7-oxo-7<i>H</i>-benzo[<i>de</i>]imidazo[5,1-<i>a</i>]isoquinoline-11-carboxylate--trifluoroacetic
 acid (1/1)
;
_journal_coeditor_code           GK2567
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o977
_journal_page_last               o978
_journal_paper_doi               10.1107/S1600536813013834
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          'C17 H12 N2 O3, C2 H F3 O2'
_chemical_formula_moiety         'C17 H12 N2 O3, C2 H F3 O2'
_chemical_formula_sum            'C19 H13 F3 N2 O5'
_chemical_formula_weight         406.31
_chemical_name_systematic
'Ethyl 7-oxo-7<i>H</i>-benzo[<i>de</i>]imidazo[5,1-<i>a</i>]isoquinoline-11-carboxylate--trifluoroacetic acid (1/1)'
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                97.539(8)
_cell_angle_beta                 98.055(8)
_cell_angle_gamma                92.695(8)
_cell_formula_units_Z            2
_cell_length_a                   7.642(3)
_cell_length_b                   8.111(4)
_cell_length_c                   14.043(6)
_cell_measurement_reflns_used    800
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.032
_cell_measurement_theta_min      2.529
_cell_volume                     852.5(6)
_computing_cell_refinement       'SAINT (Bruker, 2000)'
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_molecular_graphics
'ORTEPIII (Burnett & Johnson, 1996) and ORTEP-3 for Windows (Farrugia, 2012)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       '\f and \w scans'
_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  0.0319
_diffrn_reflns_av_sigmaI/netI    0.0410
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            7689
_diffrn_reflns_theta_full        26.16
_diffrn_reflns_theta_max         26.16
_diffrn_reflns_theta_min         2.54
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.137
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.711
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2000; Blessing, 1995)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.583
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       spike
_exptl_crystal_F_000             416
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.418
_refine_diff_density_min         -0.276
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     267
_refine_ls_number_reflns         3380
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0653
_refine_ls_R_factor_gt           0.0495
_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^)+(0.0934P)^2^+0.1240P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1284
_refine_ls_wR_factor_ref         0.1398
_reflns_number_gt                2642
_reflns_number_total             3380
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            gk2567.cif
_cod_data_source_block           I
_cod_original_cell_volume        852.6(6)
_cod_database_code               2237839
_cod_database_fobs_code          2237839