Thiobarbiturate and barbiturate salts of pefloxacin drug: Growth, structure, thermal stability and IR-spectra
N.N. Golovnev; M.S. Molokeev; M.K. Lesnikov; I.V. Sterkhova; V.V. Atuchin; Journal of Molecular Structure 1149 (2017) 367–372; doi:10.1016/j.molstruc.2017.08.011

data_1547307
_publ_section_title
;
 Thiobarbiturate and barbiturate salts of pefloxacin drug: Growth,
 structure, thermal stability and IR-spectra
;
_journal_issue                   0
_journal_name_full               'Journal of Molecular Structure'
_journal_page_first              367
_journal_page_last               372
_journal_paper_doi               10.1016/j.molstruc.2017.08.011
_journal_volume                  1149
_journal_year                    2017
_chemical_formula_moiety       'C17 H21 F N3 O3, C4 H3 N2 O3, 1.281(H2 O)'
_chemical_formula_sum            'C21 H25 F N5 O7.28'
_chemical_formula_weight         482.94
_chemical_name_systematic
;
bis(pefloxacinium 2-thiobarbiturate) hydrate
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                101.2430(10)
_cell_angle_beta                 92.5140(10)
_cell_angle_gamma                109.4710(10)
_cell_formula_units_Z            4
_cell_length_a                   10.3252(3)
_cell_length_b                   13.8631(4)
_cell_length_c                   16.9586(3)
_cell_measurement_reflns_used    24769
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.511
_cell_measurement_theta_min      2.107
_cell_volume                     2229.09(10)
_computing_cell_refinement       'APEX2 (Bruker, 2003-2008)'
_computing_data_collection       'APEX2 (Bruker, 2003-2008)'
_computing_data_reduction        'SAINT (Bruker, 2009)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2005)'
_computing_publication_material  'publCIF (Westrip, 2009)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0278
_diffrn_reflns_av_unetI/netI     0.0325
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            24769
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         27.511
_diffrn_reflns_theta_min         2.107
_exptl_absorpt_coefficient_mu    0.115
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6176
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2004/1. Bruker AXS Inc., Madison, Wisconsin, USA, 2004
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.439
_exptl_crystal_description       block
_exptl_crystal_F_000             1013
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.626
_refine_diff_density_min         -0.373
_refine_diff_density_rms         0.051
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     637
_refine_ls_number_reflns         10127
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0747
_refine_ls_R_factor_gt           0.0550
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1137P)^2^+0.3971P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1704
_refine_ls_wR_factor_ref         0.1891
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7257
_reflns_number_total             10127
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            PefH2Hba2_2p5H2O.cif
_cod_data_source_block           p3
_cod_depositor_comments
;

2019-06-28
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C42 H50 F2 N10 O14.56'
_cod_original_formula_weight         965.88
_cod_original_formula_moiety
;
2(C17 H21 F N3 O3), 2(C4 H3 N2 O3), H2 O, 1.563(O)
;
_cod_original_formula_units_Z            2
_cod_database_code               1547307
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              96678