Crystal structures of anhydrous and hydrated ceftibuten
Nisbet, Matthew L.; Puzan, Marissa; Wojtas, Lukasz; Samas, Brian; Wood, Geoffrey P. F.; Acta Crystallographica Section E 78 (2022) –; doi:10.1107/S2056989022002110

data_2244053
_publ_section_title
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 Crystal structures of anhydrous and hydrated ceftibuten
;
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2056989022002110
_journal_volume                  78
_journal_year                    2022
_chemical_absolute_configuration ad
_chemical_formula_iupac          'C15 H14 N4 O6 S2, 2.652H2 O'
_chemical_formula_moiety         'C15 H14 N4 O6 S2, 2.652(H2 O)'
_chemical_formula_sum            'C15 H19.3 N4 O8.65 S2'
_chemical_formula_weight         458.21
_chemical_name_common
;
Ceftibuten 2.652-hydrate
;
_chemical_name_systematic
'(6<i>R</i>,7<i>R</i>)-7-{[(<i>Z</i>)-2-(2-Amino-1,3-thiazol-4-yl)-4-carboxybut-2-enoyl]amino}-8-oxo-5-thia-1-azabicyclo[4.2.0]oct-2-ene-2-carboxylic acid 2.652-hydrate'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   4.66900(10)
_cell_length_b                   17.8029(4)
_cell_length_c                   23.1486(5)
_cell_measurement_reflns_used    8801
_cell_measurement_temperature    100
_cell_measurement_theta_max      77.237
_cell_measurement_theta_min      3.131
_cell_volume                     1924.15(7)
_computing_cell_refinement
;
SAINT (Bruker, 2016)
;
_computing_data_collection
;
SAINT (Bruker, 2016)
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_computing_data_reduction
;
SAINT (Bruker, 2016)
;
_computing_molecular_graphics
;
<i>OLEX2</i> (Dolomanov <i>et al.</i>,  2009)
;
_computing_publication_material
;
<i>OLEX2</i> (Dolomanov <i>et al.</i>,  2009)
;
_computing_structure_refinement
;
SHELXL  (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker D8 Venture Photon-II CPAD'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  mirrors
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0699
_diffrn_reflns_av_unetI/netI     0.0438
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            26013
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         77.965
_diffrn_reflns_theta_min         3.131
_diffrn_source                   'INCOATEC Imus micro-focus source'
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.040
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9185
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2016)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.582
_exptl_crystal_description       needle
_exptl_crystal_F_000             954
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.304
_refine_diff_density_min         -0.226
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 1302 quotients
[(<i>I</i>^+^)-(<i>I</i>^-^)]/[(<i>I</i>^+^)+(<i>I</i>^-^)]
(Parsons <i>et al.</i>,  2013)
;
_refine_ls_abs_structure_Flack   0.029(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     317
_refine_ls_number_reflns         4040
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0456
_refine_ls_R_factor_gt           0.0381
_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^)+(0.0405P)^2^+0.5445P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0824
_refine_ls_wR_factor_ref         0.0854
_reflns_number_gt                3605
_reflns_number_total             4040
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            hb8008sup1.cif
_cod_data_source_block           II
_cod_original_formula_sum        'C15 H19.30 N4 O8.65 S2'
_cod_database_code               2244053
_shelx_estimated_absorpt_t_min   0.751
_shelx_estimated_absorpt_t_max   0.942
_shelx_hkl_checksum              30244
_shelx_res_checksum              14291
_cod_database_fobs_code 2244053