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_7240153
_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_absolute_configuration syn
_chemical_formula_moiety         'C17 H19 F N3 O3, Cl'
_chemical_formula_sum            'C17 H19 Cl F N3 O3'
_chemical_formula_weight         367.81
_chemical_name_common            'Ciprfloxacin Hydrochloride Anhydrous Form I'
_chemical_name_systematic        'Ciprfloxacin Hydrochloride Anhydrous Form I'
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      61
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_audit_creation_date             2016-04-11T14:27
_audit_creation_method           'from EXP file using GSAS2CIF'
_audit_update_record
;
2020-02-06 deposited with the CCDC.	2020-03-20 downloaded from the CCDC.
;
_cell_angle_alpha                90.0
_cell_angle_beta                 90.0
_cell_angle_gamma                90.0
_cell_formula_units_Z            8
_cell_length_a                   18.1041(6)
_cell_length_b                   7.30090(17)
_cell_length_c                   26.2525(10)
_cell_measurement_temperature    298
_cell_volume                     3469.96(19)
_computing_structure_refinement  GSAS
_diffrn_ambient_pressure         101.3
_diffrn_ambient_temperature      298
_diffrn_measurement_device_type  'multiple-detector system'
_diffrn_radiation_polarisn_ratio 0.9
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     1.196212
_diffrn_source                   'synchontron, KEK, Japan'
_diffrn_source_type              'KEK PF Beam line 04B2'
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  1.00000
_exptl_absorpt_process_details
;   GSAS Absorption/surface roughness correction: function number 0
 No correction is applied.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.408
_exptl_crystal_recrystallization_method 'Heating from 1.43 Hydrate'
_pd_block_id                     2016-04-11T14:27|CPFX||
_pd_calc_method                  'Rietveld Refinement'
_pd_instr_location               ' ?'
_pd_meas_2theta_range_inc        0.01
_pd_meas_2theta_range_max        99.98
_pd_meas_2theta_range_min        1.01
_pd_meas_number_of_points        9898
_pd_phase_name                   'from C:/data/powder/PF/20140311/CPFX.cif'
_pd_proc_2theta_range_inc        0.01
_pd_proc_2theta_range_max        99.98825
_pd_proc_2theta_range_min        1.01825
_pd_proc_info_datetime           2016-04-11T14:27:02
_pd_proc_info_excluded_regions   ' ?'
_pd_proc_ls_background_function
;   GSAS Background function number 1 with 36 terms.
 Shifted Chebyshev function of 1st kind
      1:    322.789     2:   -190.403     3:    92.4369     4:   -53.5010    
      5:    41.0594     6:   -61.5204     7:    47.1743     8:   -15.4963    
      9:   -11.9148    10:    23.2382    11:  -0.351056    12:   -20.3517    
     13:    18.8221    14:   -2.72919    15:   -14.0325    16:    13.2607    
     17:  -0.694300    18:   -7.05537    19:    5.73535    20:   -1.70170    
     21:   -2.30549    22:   -1.47884    23:    2.14214    24:  -0.510942    
     25:   0.244662    26:  -0.404039    27:   -2.64398    28:   0.213078    
     29:    3.06889    30:   -2.37509    31:   0.385600    32:    1.67841    
     33:   -2.26890    34:   -1.86350    35:    5.09812    36:   -5.03861    
;
_pd_proc_ls_peak_cutoff          0.01000
_pd_proc_ls_pref_orient_corr
;   March-Dollase
 AXIS  1 Ratio=     0.844 Frac     0.968  h= 1.000  k= 1.000  l= 0.000
 AXIS  2 Ratio=     2.200 Frac     0.032  h= 0.000  k= 1.000  l= 0.000
 Prefered orientation correction range: Min=   0.82756, Max=   1.41083
;
_pd_proc_ls_profile_function
;
 CW Profile function number 3 with  19 terms
 Pseudovoigt profile coefficients as parameterized in
 P. Thompson, D.E. Cox & J.B. Hastings (1987). J. Appl. Cryst.,20,79-83.
 Asymmetry correction of L.W. Finger, D.E. Cox & A. P. Jephcoat (1994).
 J. Appl. Cryst.,27,892-900.
 #1(GU)   =  464.020 #2(GV)   =    4.633 #3(GW)   =   -1.073
 #4(GP)   =    0.100 #5(LX)   =    2.330 #6(LY)   =    0.002
 #7(S/L)  =   0.0070 #8(H/L)  =   0.0085
 #9(trns) =     0.00 #10(shft)=   0.0000
 #11(stec)=     0.00 #12(ptec)=     0.00 #13(sfec)=     0.00
 #14(L11) =    0.037 #15(L22) =    0.496 #16(L33) =    0.001
 #17(L12) =    0.156 #18(L13) =   -0.009 #19(L23) =    0.024
 Peak tails are ignored  where the intensity is below 0.0100 times the peak
   Aniso. broadening axis   0.0   0.0   1.0
;
_pd_proc_ls_prof_R_factor        0.0530
_pd_proc_ls_prof_wR_expected     0.0467
_pd_proc_ls_prof_wR_factor       0.0746
_pd_proc_number_of_points        9898
_pd_spec_mounting                ' ?'
_refine_ls_goodness_of_fit_all   1.74
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     174
_refine_ls_number_restraints     145
_refine_ls_R_Fsqd_factor         0.08626
_refine_ls_shift/su_max          0.04
_refine_ls_shift/su_mean         0.00
_reflns_d_resolution_high        1.043
_reflns_d_resolution_low         13.126
_reflns_limit_h_max              17
_reflns_limit_h_min              0
_reflns_limit_k_max              7
_reflns_limit_k_min              0
_reflns_limit_l_max              25
_reflns_limit_l_min              0
_reflns_number_total             1601
_cod_data_source_file            d0ce00261e2.cif
_cod_data_source_block           CPFX_publ
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_geom_angle_publ_flag' value 'N' was changed to 'n' 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 (85 times).

data item '_geom_bond_publ_flag' value 'N' was changed to 'n' 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 (102 times).

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_original_cell_volume        3469.95(26)
_cod_database_code               7240153
_gsas_exptl_extinct_corr_t_min   1.00000
_gsas_exptl_extinct_corr_t_max   1.00000