Bis[(2<i>R</i>,6<i>S</i>)-4-(5-amino-3-carboxy-1-cyclopropyl-6,8-difluoro-4-oxo-1,4-dihydroquinolin-7-yl)-2,6-dimethylpiperazin-1-ium] sulfate pentahydrate
Li, Tao; Yang, Lin; Wang, Yuan Cheng; Lian, Qiang; Acta Crystallographica Section E 67 (2011) o3366–o3367; doi:10.1107/S160053681104757X

data_2232787
_publ_section_title
;
 Bis[(2<i>R</i>,6<i>S</i>)-4-(5-amino-3-carboxy-1-cyclopropyl-6,8-difluoro-4-oxo-1,4-dihydroquinolin-7-yl)-2,6-dimethylpiperazin-1-ium]
 sulfate pentahydrate
;
_journal_coeditor_code           IM2333
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o3366
_journal_page_last               o3367
_journal_paper_doi               10.1107/S160053681104757X
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          '2C19 H23 F2 N4 O3 +, S O4 2-, 5H2 O'
_chemical_formula_moiety         '2(C19 H23 F2 N4 O3 +), O4 S 2-, 5(H2 O)'
_chemical_formula_sum            'C38 H56 F4 N8 O15 S'
_chemical_formula_weight         972.97
_chemical_name_systematic
;
Bis[(2<i>R</i>,6<i>S</i>)-4-(5-amino-3-carboxy-1-cyclopropyl-6,8-difluoro-
4-oxo-1,4-dihydroquinolin-7-yl)-2,6-dimethylpiperazin-1-ium] sulfate
pentahydrate
;
_space_group_IT_number           1
_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                84.760(6)
_cell_angle_beta                 83.045(5)
_cell_angle_gamma                88.619(5)
_cell_formula_units_Z            1
_cell_length_a                   7.1961(3)
_cell_length_b                   9.6892(4)
_cell_length_c                   15.6136(5)
_cell_measurement_reflns_used    3371
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.4619
_cell_measurement_theta_min      2.0779
_cell_volume                     1076.03(7)
_computing_cell_refinement       'CrystalClear (Rigaku, 2007)'
_computing_data_collection       'CrystalClear (Rigaku, 2007)'
_computing_data_reduction        'CrystalClear (Rigaku, 2007)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_device_type  'Rigaku Mercury CCD/AFC'
_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  0.0270
_diffrn_reflns_av_sigmaI/netI    0.0621
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            8268
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         2.39
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.172
_exptl_absorpt_correction_T_max  0.966
_exptl_absorpt_correction_T_min  0.966
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(CrystalClear; Rigaku, 2007)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.501
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             512
_exptl_crystal_size_max          0.2000
_exptl_crystal_size_mid          0.2000
_exptl_crystal_size_min          0.2000
_refine_diff_density_max         0.245
_refine_diff_density_min         -0.284
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.970
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     620
_refine_ls_number_reflns         6614
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.970
_refine_ls_R_factor_all          0.0434
_refine_ls_R_factor_gt           0.0386
_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^)+(0.0396P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0841
_refine_ls_wR_factor_ref         0.0858
_reflns_number_gt                5665
_reflns_number_total             6614
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            im2333.cif
_cod_data_source_block           I
_cod_original_sg_symbol_Hall     'p 1'
_cod_database_code               2232787
_cod_database_fobs_code          2232787