Crystal structure of (<i>RS</i>)-4-(3-carboxy-1-ethyl-6,8-difluoro-4-oxo-1,4-dihydroquinolin-7-yl)-2-methylpiperazin-1-ium 3-carboxy-5-fluorobenzoate
Feng, Sheng; Zhu, Gui-Liang; Sun, Jia-Jia; Chen, Chen; Zhang, Zhi-Hui; Acta Crystallographica Section E 75 (2019) 68–70; doi:10.1107/S2056989018016961

data_2242790
_publ_section_title
;
 Crystal structure of
 (<i>RS</i>)-4-(3-carboxy-1-ethyl-6,8-difluoro-4-oxo-1,4-dihydroquinolin-7-yl)-2-methylpiperazin-1-ium
 3-carboxy-5-fluorobenzoate
;
_journal_coeditor_code           WM5472
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              68
_journal_page_last               70
_journal_paper_doi               10.1107/S2056989018016961
_journal_volume                  75
_journal_year                    2019
_chemical_formula_iupac          'C17 H20 F2 N3 O3 +, C8 H4 F O4 -'
_chemical_formula_moiety         'C17 H20 F2 N3 O3 +, C8 H4 F O4 -'
_chemical_formula_sum            'C25 H24 F3 N3 O7'
_chemical_formula_weight         535.47
_chemical_name_systematic
'(<i>RS</i>)-4-(3-Carboxy-1-ethyl-6,8-difluoro-4-oxo-1,4-dihydroquinolin-7-yl)-2-methylpiperazin-1-ium 3-carboxy-5-fluorobenzoate'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 100.707(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.4324(12)
_cell_length_b                   16.5656(19)
_cell_length_c                   14.0448(17)
_cell_measurement_reflns_used    5522
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      29.93
_cell_measurement_theta_min      2.24
_cell_volume                     2385.0(5)
_computing_cell_refinement
;
SAINT (Bruker, 2010)
;
_computing_data_collection
;
APEX2 (Bruker, 2010)
;
_computing_data_reduction
;
SAINT (Bruker, 2010)
;
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.877
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0347
_diffrn_reflns_av_unetI/netI     0.0428
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            16570
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.357
_diffrn_reflns_theta_min         1.921
_exptl_absorpt_coefficient_mu    0.125
_exptl_absorpt_correction_T_max  0.980
_exptl_absorpt_correction_T_min  0.970
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>SADABS</i>; Bruker, 2010)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.491
_exptl_crystal_description       block
_exptl_crystal_F_000             1112
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.160
_refine_diff_density_max         0.292
_refine_diff_density_min         -0.279
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.978
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     358
_refine_ls_number_reflns         6292
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.978
_refine_ls_R_factor_all          0.0831
_refine_ls_R_factor_gt           0.0541
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0850P)^2^+0.6860P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1417
_refine_ls_wR_factor_ref         0.1612
_reflns_number_gt                4335
_reflns_number_total             6292
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            wm5472sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        2384.9(5)
_cod_database_code               2242790
_cod_database_fobs_code          2242790
_shelx_estimated_absorpt_t_min   0.973
_shelx_estimated_absorpt_t_max   0.980
_shelx_hkl_checksum              91980
_shelx_res_checksum              805
_shelxl_version_number           2014/6