4-(3-Carboxy-1-ethyl-6-fluoro-4-oxo-1,4-dihydroquinolin-7-yl)piperazin-1-ium 4-carboxybenzoate–benzene-1,4-dicarboxylic acid (2/1)
Yan, Shi-Wei; Chen, Hai-Yan; Zhang, Guang-Ju; Liao, Qin; Liang, Yan-Chen; Acta Crystallographica Section E 67 (2011) o909–; doi:10.1107/S1600536811009524

data_2229635
_publ_section_title
;
 4-(3-Carboxy-1-ethyl-6-fluoro-4-oxo-1,4-dihydroquinolin-7-yl)piperazin-1-ium
 4-carboxybenzoate--benzene-1,4-dicarboxylic acid (2/1)
;
_journal_coeditor_code           FF2003
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o909
_journal_paper_doi               10.1107/S1600536811009524
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          '2C16 H19 F N3 O3 +, 2C8 H5 O4 -, C8 H6 O4'
_chemical_formula_moiety         '2(C16 H19 F N3 O3 +), 2(C8 H5 O4 -), C8 H6 O4'
_chemical_formula_sum            'C56 H54 F2 N6 O18'
_chemical_formula_weight         1137.06
_chemical_name_systematic
;
4-(3-Carboxy-1-ethyl-6-fluoro-4-oxo-1,4-dihydroquinolin-7-yl)piperazin-1-ium
4-carboxybenzoate--benzene-1,4-dicarboxylic acid (2/1)
;
_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                89.304(2)
_cell_angle_beta                 74.672(2)
_cell_angle_gamma                71.677(2)
_cell_formula_units_Z            1
_cell_length_a                   9.8901(15)
_cell_length_b                   10.2420(16)
_cell_length_c                   13.665(2)
_cell_measurement_reflns_used    10704
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.43
_cell_measurement_theta_min      2.51
_cell_volume                     1263.5(3)
_computing_cell_refinement       'SAINT (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT (Bruker, 2001)'
_computing_molecular_graphics    'SHELXTL-Plus (Sheldrick, 2008)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker APEX CCD area-detector'
_diffrn_measurement_method       '\f and \w'
_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  0.0239
_diffrn_reflns_av_sigmaI/netI    0.0325
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            10704
_diffrn_reflns_theta_full        26.43
_diffrn_reflns_theta_max         26.43
_diffrn_reflns_theta_min         2.51
_exptl_absorpt_coefficient_mu    0.117
_exptl_absorpt_correction_T_max  0.9590
_exptl_absorpt_correction_T_min  0.9480
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            ' yellow'
_exptl_crystal_density_diffrn    1.494
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             594
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.36
_refine_diff_density_max         0.257
_refine_diff_density_min         -0.277
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     394
_refine_ls_number_reflns         5143
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.0545
_refine_ls_R_factor_gt           0.0419
_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^)+(0.0950P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1255
_refine_ls_wR_factor_ref         0.1369
_reflns_number_gt                4031
_reflns_number_total             5143
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ff2003.cif
_cod_data_source_block           I
_cod_depositor_comments
;

2019-10-14
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_moiety     'C16 H19 F N3 O3 +, C8 H5 O4 -, 0.5(C8 H6 O4)'
_cod_original_formula_iupac      'C16 H19 F N3 O3 +, C8 H5 O4 -, 0.5C8 H6 O4'
_cod_original_formula_sum        'C28 H27 F N3 O9'
_cod_original_formula_units_Z    2
_cod_original_formula_weight     568.53
_cod_database_code               2229635
_cod_database_fobs_code          2229635