Azilsartan piperazine salt solvate and monohydrate: preparation, crystal structure, enhanced solubility and oral bioavailability
Xu, Juan; Du, Rongkai; Wu, Lvying; Zhang, Xianrui; Guan, Su; Zhang, Lei; Ning, Lifeng; Li, Shan; New Journal of Chemistry 44 (2020) 852–860; doi:10.1039/C9NJ05042F

data_7059191
_publ_section_title
;
 Azilsartan piperazine salt solvate and monohydrate: preparation, crystal
 structure, enhanced solubility and oral bioavailability
;
_journal_issue                   3
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              852
_journal_page_last               860
_journal_paper_doi               10.1039/C9NJ05042F
_journal_volume                  44
_journal_year                    2020
_chemical_formula_moiety         'C25 H19 N4 O5, 1/2 C4 H12 N2, C2 H6 O'
_chemical_formula_sum            'C29 H31 N5 O6'
_chemical_formula_weight         545.59
_chemical_name_common            'Azilsartan-Piperazine-ethanol '
_chemical_name_systematic
; 
 '2-Ethoxy-1-[[2??-(4,5-dihydro-5-oxo-1,2,4-oxadiazol-3-yl)biphenyl-4-yl]methyl]benzimidazole-7-carboxylic acid?\/c2-ethoxy-3-((2'-(5-oxo-2,5-dihydro-1,2,4-oxadiazol-3-yl)biphenyl-4-yl)Methyl)-3H-benzozimidazole-4-carboxylic acid:Piperazine:ethanol(1:0.5:1) ' 
;
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -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_block_doi                 10.5517/ccdc.csd.cc1phhwk
_audit_creation_method           SHELXL-97
_audit_update_record
;
2017-07-24 deposited with the CCDC.	2019-12-09 downloaded from the CCDC.
;
_cell_angle_alpha                82.781(8)
_cell_angle_beta                 85.788(7)
_cell_angle_gamma                89.002(7)
_cell_formula_units_Z            2
_cell_length_a                   5.7924(4)
_cell_length_b                   13.4728(13)
_cell_length_c                   17.3811(18)
_cell_measurement_reflns_used    10975
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      25.02
_cell_measurement_theta_min      2.97
_cell_volume                     1342.0(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEXII CCD area-detector'
_diffrn_measurement_method       '\f and \w'
_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  0.0319
_diffrn_reflns_av_sigmaI/netI    0.0691
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            9179
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         2.97
_exptl_absorpt_coefficient_mu    0.096
_exptl_absorpt_correction_T_max  0.9699
_exptl_absorpt_correction_T_min  0.9671
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.350
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             576
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.32
_refine_diff_density_max         0.209
_refine_diff_density_min         -0.331
_refine_diff_density_rms         0.043
_refine_ls_extinction_coef       0.009(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     372
_refine_ls_number_reflns         4720
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0958
_refine_ls_R_factor_gt           0.0570
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0742P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1404
_refine_ls_wR_factor_ref         0.1672
_reflns_number_gt                2983
_reflns_number_total             4720
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c9nj05042f1.cif
_cod_data_source_block           exp_2847
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Triclinic' was changed to
'triclinic' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 

 Adding full bibliography for 7059191--7059193.cif.

 Adding full bibliography for 7059191--7059193.cif.
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7059191