Structural Origin of Physicochemical Properties Differences upon Dehydration and Polymorphic Transformation of Ciprofloxacin Hydrochloride Revealed by Structure Determination from Powder X-ray Diffraction Data
Putra, Okky Dwichandra; Pettersen, Anna; Yonemochi, Etsuo; Uekusa, Hidehiro; CrystEngComm  (2020) –; doi:10.1039/D0CE00261E

data_7240151
_publ_section_title
;
 Structural Origin of Physicochemical Properties Differences upon
 Dehydration and Polymorphic Transformation of Ciprofloxacin Hydrochloride
 Revealed by Structure Determination from Powder X-ray Diffraction Data
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D0CE00261E
_journal_year                    2020
_chemical_formula_moiety         'C17 H19 F N3 O3, 0.215(H4 O2), Cl, H2 O'
_chemical_formula_sum            'C17 H21.86 Cl F N3 O4.43'
_chemical_formula_weight         393.56
_chemical_name_common            'Ciprofloxacin Hydrochloride 1.43 Hydrate'
_chemical_name_systematic        'Ciprofloxacin Hydrochloride 1.43 Hydrate'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yab'
_space_group_name_H-M_alt        'P 1 21/a 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2020-02-06 deposited with the CCDC.	2020-03-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.7338(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.02521(13)
_cell_length_b                   19.6681(4)
_cell_length_c                   12.9331(2)
_cell_measurement_reflns_used    20568
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      68.206
_cell_measurement_theta_min      3.418
_cell_volume                     1786.85(6)
_computing_cell_refinement       RAPID-AUTO
_computing_data_collection       RAPID-AUTO
_computing_data_reduction        RAPID-AUTO
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 10.0
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'RIGAKU R-AXIS RAPID II'
_diffrn_measurement_method       \w-scan
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54186
_diffrn_reflns_av_R_equivalents  0.0302
_diffrn_reflns_av_unetI/netI     0.0174
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            20568
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.686
_diffrn_reflns_theta_max         68.206
_diffrn_reflns_theta_min         3.418
_diffrn_source                   'rotating anode X-ray'
_exptl_absorpt_coefficient_mu    2.271
_exptl_absorpt_correction_T_max  0.869
_exptl_absorpt_correction_T_min  0.657
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'abscor, T.Higashi RIGAKU'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.463
_exptl_crystal_description       needle
_exptl_crystal_F_000             825
_exptl_crystal_size_max          0.115
_exptl_crystal_size_mid          0.095
_exptl_crystal_size_min          0.062
_refine_diff_density_max         0.487
_refine_diff_density_min         -0.373
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     268
_refine_ls_number_reflns         3247
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0413
_refine_ls_R_factor_gt           0.0388
_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^)+(0.0597P)^2^+0.7477P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1040
_refine_ls_wR_factor_ref         0.1068
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2976
_reflns_number_total             3247
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ce00261e2.cif
_cod_data_source_block           shelx
_cod_original_sg_symbol_H-M      'P 21/a'
_cod_database_code               7240151
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.780
_shelx_estimated_absorpt_t_max   0.872
_shelx_res_checksum              20668