Novel pharmaceutical salts of cephalexin with organic counterions: structural analysis and properties
Hua, Xiu-Ni; Pan, Xia; Zhu, Yang; Cai, Zhuoer; Song, Qi; Li, Yaozhenhui; Feng, Wenbin; Chen, Xin; Zhang, Hui; Sun, Baiwang; RSC Advances 12 (2022) 34843–34850; doi:10.1039/D2RA05565A

data_7245978
_publ_section_title
;
 Novel pharmaceutical salts of cephalexin with organic counterions:
 structural analysis and properties
;
_journal_issue                   54
_journal_name_full               'RSC Advances'
_journal_page_first              34843
_journal_page_last               34850
_journal_paper_doi               10.1039/D2RA05565A
_journal_volume                  12
_journal_year                    2022
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C16 H18 N3 O4 S, C7 H5 O6 S, 4(H2 O)'
_chemical_formula_sum            'C23 H31 N3 O14 S2'
_chemical_formula_weight         637.63
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2022-10-29 deposited with the CCDC.	2022-11-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.464(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.7579(9)
_cell_length_b                   7.0785(3)
_cell_length_c                   27.0868(16)
_cell_measurement_reflns_used    6567
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.12
_cell_measurement_theta_min      2.28
_cell_volume                     2805.6(3)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       'Bruker APEX-II CCD diffractometer'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'DIAMOND (Brandenburg & Putz, 2005)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.992
_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  0.0896
_diffrn_reflns_av_unetI/netI     0.0633
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            55635
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.424
_diffrn_reflns_theta_min         1.921
_exptl_absorpt_coefficient_mu    0.265
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6958
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2016/2 (Bruker,2016/2)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.510
_exptl_crystal_description       strip
_exptl_crystal_F_000             1336
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.587
_refine_diff_density_min         -0.422
_refine_diff_density_rms         0.076
_refine_ls_abs_structure_details
;
 Flack x determined using 3985 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.01(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.149
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     767
_refine_ls_number_reflns         11413
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.150
_refine_ls_R_factor_all          0.0639
_refine_ls_R_factor_gt           0.0567
_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^)+(0.0540P)^2^+1.6634P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1241
_refine_ls_wR_factor_ref         0.1280
_reflns_Friedel_coverage         0.840
_reflns_Friedel_fraction_full    0.988
_reflns_Friedel_fraction_max     0.987
_reflns_number_gt                10360
_reflns_number_total             11413
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ra05565a2.cif
_cod_data_source_block           1_CCDC2
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7245978
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.949
_shelx_estimated_absorpt_t_max   0.974
_shelx_res_checksum              18308