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_7245977
_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 H4 Cl O3, 1.5(H2 O)'
_chemical_formula_sum            'C23 H25 Cl N3 O8.5 S'
_chemical_formula_weight         546.97
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 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                 95.3770(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   30.1649(13)
_cell_length_b                   7.7132(3)
_cell_length_c                   10.9391(4)
_cell_measurement_reflns_used    7225
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.35
_cell_measurement_theta_min      2.73
_cell_volume                     2533.98(17)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_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 0.989
_diffrn_measured_fraction_theta_max 0.989
_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  0.0424
_diffrn_reflns_av_unetI/netI     0.0387
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            18174
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.393
_diffrn_reflns_theta_min         2.726
_exptl_absorpt_coefficient_mu    0.288
_exptl_absorpt_correction_T_max  0.972
_exptl_absorpt_correction_T_min  0.949
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2016/2 (Bruker,2016/2)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.434
_exptl_crystal_description       strip
_exptl_crystal_F_000             1140
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.332
_refine_diff_density_min         -0.322
_refine_diff_density_rms         0.055
_refine_ls_abs_structure_details
;
 Flack x determined using 1876 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   1.091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         5090
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0523
_refine_ls_R_factor_gt           0.0472
_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^)+(0.0732P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1124
_refine_ls_wR_factor_ref         0.1164
_reflns_Friedel_coverage         0.832
_reflns_Friedel_fraction_full    0.967
_reflns_Friedel_fraction_max     0.961
_reflns_number_gt                4571
_reflns_number_total             5090
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ra05565a2.cif
_cod_data_source_block           1_CCDC1
_cod_depositor_comments
;

2025-04-02
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C46 H50 Cl2 N6 O17 S2'
_cod_original_formula_weight         1093.94
_cod_original_formula_moiety     '2(C16 H18 N3 O4 S), 2(C7 H4 Cl O3), 3(H2 O)'
_cod_original_formula_units_Z            2
_cod_original_sg_symbol_H-M      'C 2'
_cod_database_code               7245977
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.945
_shelx_estimated_absorpt_t_max   0.972
_shelx_res_checksum              53905