6-Ethoxycarbonyl-5,7-dihydroxy-2,3-dihydro-1<i>H</i>-pyrido[3,2,1-<i>ij</i>]quinolinium tribromide
Rybakov, Victor B.; Shishkina, Svitlana V.; Ukrainets, Igor V.; Golik, Nikolai Yu.; Chernenok, Igor N.; Acta Crystallographica Section E 69 (2013) o82–; doi:10.1107/S1600536812049276

data_2237106
_publ_section_title
;
 6-Ethoxycarbonyl-5,7-dihydroxy-2,3-dihydro-1<i>H</i>-pyrido[3,2,1-<i>ij</i>]quinolinium
 tribromide
;
_journal_coeditor_code           AA2080
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o82
_journal_paper_doi               10.1107/S1600536812049276
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          'C15 H16 N O4 + , Br3 -'
_chemical_formula_moiety         'C15 H16 N O4 +, Br3 -'
_chemical_formula_sum            'C15 H16 Br3 N O4'
_chemical_formula_weight         513.99
_chemical_melting_point_gt       360
_chemical_melting_point_lt       362
_chemical_name_systematic
;
6-Ethoxycarbonyl-5,7-dihydroxy-2,3-dihydro-1<i>H</i>-
pyrido[3,2,1-<i>ij</i>]quinolinium tribromide
;
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                102.355(9)
_cell_angle_beta                 98.777(9)
_cell_angle_gamma                98.093(9)
_cell_formula_units_Z            2
_cell_length_a                   7.6491(8)
_cell_length_b                   9.1729(10)
_cell_length_c                   13.3722(14)
_cell_measurement_reflns_used    1363
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      32.04
_cell_measurement_theta_min      3.10
_cell_volume                     891.05(17)
_computing_cell_refinement       'CrysAlis RED (Agilent, 2011)'
_computing_data_collection       'CrysAlis CCD (Agilent, 2011)'
_computing_data_reduction        'CrysAlis RED (Agilent, 2011)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      295(2)
_diffrn_detector_area_resol_mean 16.1827
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Agilent Xcalibur-3 CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-Ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0338
_diffrn_reflns_av_sigmaI/netI    0.0671
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            10147
_diffrn_reflns_theta_full        29.99
_diffrn_reflns_theta_max         29.99
_diffrn_reflns_theta_min         3.10
_exptl_absorpt_coefficient_mu    6.808
_exptl_absorpt_correction_T_max  0.7271
_exptl_absorpt_correction_T_min  0.3429
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(CrysAlis RED; Agilent, 2011)'
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.916
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             500
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.018
_refine_diff_density_min         -0.736
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.895
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     224
_refine_ls_number_reflns         5106
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      0.895
_refine_ls_R_factor_all          0.1900
_refine_ls_R_factor_gt           0.0676
_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^)+(0.1080P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1749
_refine_ls_wR_factor_ref         0.2171
_reflns_number_gt                1855
_reflns_number_total             5106
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            aa2080.cif
_cod_data_source_block           I
_cod_original_cell_volume        891.06(17)
_cod_database_code               2237106
_cod_database_fobs_code          2237106